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deuterophosphorous acid
B
[D3]phosphoric acid
Conditions | Yield |
---|---|
In dimethyl sulfoxide Kinetics; React. between 298 and 318 K.; Monitored spectrophotometrically at 356 nm.; |
Conditions | Yield |
---|---|
formation from diluted (2)H2SO4 and Ba3(PO4)2;; |
tert.-butylhydroperoxide
phosphorous
water-d2
A
trideutero hypophosphorous acid
B
deuterophosphorous acid
C
[D3]phosphoric acid
Conditions | Yield |
---|---|
In water-d2; toluene Kinetics; Ar, P4 (or soln. of P4 in toluene) added in small portions, heated to 25-60°C, stirred for 0.5-4 h; not isolated, detected by NMR; | |
In tetrahydrofuran; water-d2 Kinetics; Ar, P4 added in small portions, heated to 60°C, stirred for 0.5-4h; not isolated, detected by NMR; | |
In tetrachloromethane; water-d2 Kinetics; Ar, P4 added in small portions, heated to 60°C, stirred for 0.5-4h; not isolated, detected by NMR; | |
In hexane; water-d2 Kinetics; Ar, P4 added in small portions, heated to 60°C, stirred for 0.5-4h; not isolated, detected by NMR; | |
In water-d2 Kinetics; Ar, P4 added in small portions, heated to 90°C, stirred for 0.5-4h; not isolated, detected by NMR; |
phosphorous
dihydrogen peroxide
water-d2
A
trideutero hypophosphorous acid
B
deuterophosphorous acid
C
[D3]phosphoric acid
Conditions | Yield |
---|---|
In water-d2 Kinetics; Ar, P4 added in small portions, heated to 25-90°C, stirred for 0.5-4 h; not isolated, detected by NMR; |
phosphorous
water-d2
dibenzoyl peroxide
A
trideutero hypophosphorous acid
B
deuterophosphorous acid
C
[D3]phosphoric acid
Conditions | Yield |
---|---|
In water-d2; toluene Kinetics; Ar, P4 (or soln. of P4 in toluene) added in small portions, heated to 60-60°C, stirred for 0.5-4 h; not isolated, detected by NMR; | |
copper diacetate In water-d2; toluene Kinetics; Ar, P4 added in small portions, heated to 60°C, stirred for 0.5-4h; not isolated, detected by NMR; | |
copper(l) iodide In water-d2; toluene Kinetics; Ar, P4 added in small portions, heated to 60°C, stirred for 0.5-4h; not isolated, detected by NMR; |
Conditions | Yield |
---|---|
stoich. amts.; | |
In neat (no solvent) | |
In water-d2 P-compd. dissoln.; |
water-d2
trichlorophosphate
[D3]phosphoric acid
Conditions | Yield |
---|---|
In neat (no solvent) formation of diluted soln. with POCl3 and excess (2)H2O;; |
Conditions | Yield |
---|---|
In water-d2 |
Conditions | Yield |
---|---|
In water sublimated P4O10 converted with ultrapure D2O in moisturizing apparatus; filtered through G5 sintered glass frit under CO2-free atmosphere; |
deuterophosphorous acid
B
[D3]phosphoric acid
Conditions | Yield |
---|---|
In dimethyl sulfoxide Kinetics; react. of (2)HP(O)(O(2)H)2 with O2CrOCl at 298 K; detd. spectrophotometrically; |
Conditions | Yield |
---|---|
In ethyl [2]alcohol Reflux with stirring for 11 days;; filtered, solid was washed with D2O, dried in vac. at 60°C for 16 h; elem. anal.;; | 98.8% |
Conditions | Yield |
---|---|
In tetrahydrofuran; water-d2 D3PO4 in D2O added to a soln. of Cr complex in THF, stirred for 45 min; evapd. (vac.), sublimed; | 54% |
Conditions | Yield |
---|---|
With {18}crown-6 In tetrahydrofuran Ru-compd., NaBH4 and (18)crown-6 in THF stirred for 2.5 h at room temp., addn. of D3PO4, stirred for 5 min; excess D3PO4 neutralized with NaHCO3, dried with MgSO4, filtered, removal of solvent in vac., dissolved in CH2Cl2, TLC (hexane/CH2Cl2 7:3); | 30% |
potassium tetracarbonylcobaltate
[D3]phosphoric acid
Conditions | Yield |
---|---|
With CH2CHCH2CHCH2 In not given mechanism discussed;; | A n/a B 10% |
With CH2CHCH2CHCH2 In not given mechanism discussed;; | A n/a B 10% |
potassium tetracarbonylcobaltate
1,4-Pentadiene
water-d2
[D3]phosphoric acid
Conditions | Yield |
---|---|
In water-d2 mechanism discussed;; | A n/a B 5% |
In water-d2 mechanism discussed;; | A n/a B 5% |
Conditions | Yield |
---|---|
In neat (no solvent) vac. system.; | |
In neat (no solvent) action of perdeuterophosphoric acid on potassium cyanide in vac.; | |
With P2O5 In neat (no solvent) action of D3PO4 (with excess P2O5 added) on KCN in vac.; |
potassium carbonate
[D3]phosphoric acid
deuterated potassium dihydrogen phosphate
Conditions | Yield |
---|---|
prior synthesis carbonate dehydration for 2 h at 150°C; |
Conditions | Yield |
---|---|
In neat (no solvent) mixing (excess of NaN3); not pure; mass spectroscopy; | |
In further solvent(s) NaN3 reacted with excess D3PO4 under vac.; mass spectrum; | |
distn., FTIR anal. of purity; |
Conditions | Yield |
---|---|
adding H3PO4 to KC(15)N in vac., condensing gas evolved; |
Conditions | Yield |
---|---|
In water-d2 reaction of P-compd. soln. with Fe-compd. in deuterated vac. line; |
Conditions | Yield |
---|---|
In water-d2 condensing (-196°C, on a vac. line); vac. distn. (-20°C); |
Conditions | Yield |
---|---|
In water-d2 slow addn. of NaCN/D2O to stirred soln. of (2)H3PO4/D2O; dried (P2O5); | |
In water-d2 in vac.; trap-to-trap distn.; |
Conditions | Yield |
---|---|
In neat (no solvent) distillation of DCOONa with an excess of D3PO4;; |
Conditions | Yield |
---|---|
In water-d2 vac.; vapor condensation, distillation; | |
In not given byproducts: D2O; distn.; |
[D3]phosphoric acid
deuterated rubidium dihydrogen phosphate
Conditions | Yield |
---|---|
prior synthesis carbonate dehydration for 2 h at 350°C; | |
byproducts: CO2, D2O; | |
byproducts: D2O, CO2; | |
byproducts: (2H)2O, CO2; |
ammonium-d4 deuteroxide
[D3]phosphoric acid
deuterated ammonium dihydrogen phosphate
Conditions | Yield |
---|---|
byproducts: D2O; |
Conditions | Yield |
---|---|
In 1,4-dioxane 3 fold 3 h heating of Fe(C5H5)2 with 10 fold excess of (2)H3PO4 in abs. dioxane at 110-120°C;; 98.1 % deuterated Fe(C5H5)2;; |
[D3]phosphoric acid
deuterated potassium dihydrogen phosphate
Conditions | Yield |
---|---|
In further solvent(s) high-vacuum line; |
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