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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → Acetamide, 2-(diphenylphosphinothioyl)-N,N-diethyl-

HRID 1371243
ノート
印刷プレビュー

反応式

HRID 1371243 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.[CH2:15]([N:17]([CH2:22][CH3:23])[C:18](=[O:21])[CH2:19]Cl)[CH3:16].[OH-].[K+].O>C(Cl)Cl>[CH2:15]([N:17]([CH2:22][CH3:23])[C:18]([CH2:19][P:7](=[S:14])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)=[O:21])[CH3:16]
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 14797Potassium HydroxideHCID 16844Chloro-N,N-diethylacetamideHCID 178528040HCID 178528040、化合物

生成物 1

HCID 796778Acetamide, 2-(diphenylphosphinothioyl)-N,N-diethyl-

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A stirred mixture of diphenylphosphine sulfide (4.365 g, 0.02 mol) and N,N-diethylchloroacetamide (4.189 g, 0.028 mol) in methylene chloride (80 ml) was cooled to 8–10° C. in an ice-water bath. Small pieces of solid potassium hydroxide (3.927 g, 0.07 mol) were added while stirring under nitrogen atmosphere. After 30 minutes, water (25 ml) was added and the organic layer was separated, washed with more water (25 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 3.5 g (53%) of large cubes. mp: 108–110° 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 (25 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 3.5 g (53%) of large cubes

出典と根拠

ORDレコード
ord-415fe52e9f254e298e86d93ccb87466a
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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