Ammonia → HCID 18780196, 화합물

HRID 1421657노트

반응식

HRID 1421657 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

HCID 18780196HCID 18780196, 화합물수율 84%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-314582d17d294397bfabf6b56e9b06ce
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06077968

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