Nitrogen → HCID 20474990, compound

HRID 2295254Notes

Reaction equation

HRID 2295254 reaction equation
[P:1]([Cl:4])(Cl)Cl.[CH2:5]([O:9][C:10](=[O:17])[C:11]([CH2:15][OH:16])([CH2:13][OH:14])[CH3:12])[CH2:6][CH2:7][CH3:8].O.N#N>C1(C)C=CC=CC=1>[Cl:4][P:1]1[O:14][CH2:13][C:11]([CH3:12])([C:10]([O:9][CH2:5][CH2:6][CH2:7][CH3:8])=[O:17])[CH2:15][O:16]1

Participants

6

Reactant 4

HCID 947NitrogenHCID 962WaterHCID 24387Phosphorus trichlorideHCID 53816742HCID 53816742, compound

Product 1

HCID 20474990HCID 20474990, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

68.70 g (0.50 mol) of phosphorus trichloride in 50 ml of toluene were added dropwise with vigorous stirring, in the course of 1 hour, to a solution of 95.15 g (0.50 mol) of 2,2-bis-hydroxymethylpropionic acid butyl ester in 250 ml of toluene at 5°-10° C. The reaction mixture was subsequently stirred for 1 hour without cooling in a water-jet vacuum, during which time a gentle flow of N2 was fed in; the solvent was then distilled off in vacuo (bath temperature=50° C./15-20 mm Hg), and the residue was purified by vacuum distillation. The product obtained was in the form of a colourless liquid; nD20 =1.4701; b.p. 113°-115° C./0.1 mm Hg.

Workup

  1. distillationthe solvent was then distilled off in vacuo (bath temperature=50° C./15-20 mm Hg)
  2. distillationthe residue was purified by vacuum distillation
  3. customThe product obtained

Sources & evidence

ORD record
ord-1e659c712fff45888f706585a10b0cc9
Source dataset
uspto-grants-1984_01
Patent number
US04424173

Reaction notes

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