Ammonia → HCID 18780196, compound

HRID 725257Notes

Reaction equation

HRID 725257 reaction equation
[CH2:1]([OH:3])[CH3:2].[F:4][C:5]1[CH:10]=[CH:9][C:8]([P:11]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)Cl)=[CH:7][CH:6]=1.N>>[F:19][C:16]1[CH:17]=[CH:18][C:13]([P:11]([C:8]2[CH:9]=[CH:10][C:5]([F:4])=[CH:6][CH:7]=2)[O:3][CH2:1][CH3:2])=[CH:14][CH:15]=1

Participants

4

Reactant 3

HCID 222AmmoniaHCID 702EthanolHCID 4379931BIS(4-FLUOROPHENYL)CHLOROPHOSPHINE

Product 1

HCID 18780196HCID 18780196, compoundYield 84%

Procedure

87 g (1.90 mol) of absolute ethanol are cooled to -15° C. under a nitrogen atmosphere. 67 g (0.26 mol) of bis-(4-fluorophenyl)chlorophosphine are then added dropwise at this temperature in 50 minutes with vigorous stirring. 5.2 g (0.31 mol) of ammonia gas are then introduced at this temperature. The mixture is then further stirred until room temperature is reached and stirred for a further 16 hours. The mixture is then filtered by suction and rinsed out with ethanol. The filtrate is freed from ethanol and excess ammonia in vacuo. The remaining residue is distilled at 0.45 mbar at an overhead temperature of 102° C. 58 g of ethyl bis-(4-fluorophenyl)-phosphinite are obtained. This corresponds to a yield of 84% of theory.

Workup

  1. stirringstirred for a further 16 hours
  2. filtrationThe mixture is then filtered by suction
  3. washrinsed out with ethanol
  4. distillationThe remaining residue is distilled at 0.45 mbar at an overhead temperature of 102° C

Sources & evidence

ORD record
ord-760717fec2154fde961dd434b506f0e0
Source dataset
uspto-grants-1998_01
Patent number
US05705669

Reaction notes

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