Ammonia → HCID 18780196、化合物

HRID 725257ノート

反応式

HRID 725257 の反応式
[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

参加物

4

反応物 3

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

生成物 1

HCID 18780196HCID 18780196、化合物収率 84%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-760717fec2154fde961dd434b506f0e0
出典データセット
uspto-grants-1998_01
特許番号
US05705669

反応ノート

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