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Water → Ethanone, 2-(diphenylphosphinothioyl)-1-phenyl-

HRID 1371244
ノート
印刷プレビュー

反応式

HRID 1371244 の反応式
[C:1]1([PH:7](=[S:14])[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:16][C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[O:18].[OH-].[K+].O>C(Cl)Cl>[C:19]1([C:17]([CH2:16][P:7](=[S:14])([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[O:18])[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 107572-ChloroacetophenoneHCID 14797Potassium HydroxideHCID 178528040HCID 178528040、化合物

生成物 1

HCID 614971Ethanone, 2-(diphenylphosphinothioyl)-1-phenyl-

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A stirred mixture of diphenylphosphine sulfide (0.218 g, 0.001 mol) and chloroacetophenone (0.216 g, 0.0014 mol) in methylene chloride (4 ml) was cooled to 8–10° C. in an ice-water bath. Small pieces of solid potassium hydroxide (0.196 g, 0.0035 mol) were added while stirring under nitrogen atmosphere. After 45 minute, water (2 ml) was added and the organic layer was separated, washed with more water (2 ml) and dried over sodium sulfate. The solvent was removed under reduced pressure using a rotary evaporator and the oily residue was crystallized from ethyl acetate-hexane mixture to give 0.19 g (56.5%) of star shaped crystals. mp=83–84° C.

後処理

  1. temperaturewas cooled to 8–10° C. in an ice-water bath
  2. customthe organic layer was separated
  3. washwashed with more water (2 ml)
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customa rotary evaporator
  7. customthe oily residue was crystallized from ethyl acetate-hexane mixture
  8. customto give 0.19 g (56.5%) of star

出典と根拠

ORDレコード
ord-d9125d3c4a3b428e8432974472c5764b
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157219B2

反応ノート

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