ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

Ethanol → N-(4-amino-2-methylphenyl)-2-chloroacetamide

HRID 35324
ノート
印刷プレビュー

反応式

HRID 35324 の反応式
S1C=CC=C1.C(O)C.[Cl:9][CH2:10][C:11]([NH:13][C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-])=O)=[CH:16][C:15]=1[CH3:23])=[O:12].[H][H]>[Pt].CO>[NH2:20][C:17]1[CH:18]=[CH:19][C:14]([NH:13][C:11](=[O:12])[CH2:10][Cl:9])=[C:15]([CH3:23])[CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 702EthanolHCID 8030ThiopheneHCID 3522982-chloro-N-(2-methyl-4-nitrophenyl)acetamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 21295679N-(4-amino-2-methylphenyl)-2-chloroacetamide収率 92%

試薬・触媒・溶媒 2

HCID 23939Platinum触媒
HCID 887
Methanol
溶媒

実験手順

To 1 part of a solution of 2 parts of thiophene in 40 parts of ethanol were added 15 parts of 2-chloro-N-(2-methyl-4-nitrophenyl)acetamide and 400 parts of methanol. The whole was hydrogenated at normal pressure and at room temperature with 2 parts of platinum-on-charcoal catalyst 5%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The solid residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was suspended in 2,2'-oxybispropane. The product was filtered off and dried, yielding 12 parts (92%)of N-(4-amino-2-methylphenyl)-2-chloroacetamide (intermediate 70).

後処理

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customThe solid residue was purified by column-chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated
  7. filtrationThe product was filtered off
  8. customdried

出典と根拠

ORDレコード
ord-9a978e6b54644696a6d3ec32141b02be
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04766125

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート