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

Hydrazine hydrate (1:1) → HCID 23458522、化合物

HRID 1679925
ノート
印刷プレビュー

反応式

HRID 1679925 の反応式
O.NN.[N+:4]([C:7]1[CH:8]=[C:9]([C:13]2[CH:14]3[CH:16]([C:17](=[O:20])[NH:18][N:19]=2)[CH2:15]3)[CH:10]=[CH:11][CH:12]=1)([O-])=O>C(O)C.[Ni]>[NH2:4][C:7]1[CH:8]=[C:9]([C:13]2[CH:14]3[CH:16]([C:17](=[O:20])[NH:18][N:19]=2)[CH2:15]3)[CH:10]=[CH:11][CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 234585112-(m-Nitrophenyl)-3,4-diazabicyclo[4.1.0]hept-2-en-5-one

生成物 1

HCID 23458522HCID 23458522、化合物収率 76.5%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒2 回

実験手順

A solution of 0.65 g (13.0 millimoles) of hydrazine hydrate in 10 ml of ethanol is added, whilst stirring, to a mixture of 1.5 g (6.5 millimoles) of 2-(m-nitrophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one (see Example 32b), 20 ml of ethanol and a small amount of an aqueous Raney nickel suspension in the course of 5 minutes, during which the temperature rises from 25° to 35° C. Stirring is continued for 1 hour and the reaction mixture is then slowly raised to the boil. It is refluxed for 5 minutes and filtered hot, and the filtrate is concentrated. After recrystallization from ethyl acetate/methanol, 1.0 g (76% of theory) of 2-(m-aminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one is obtained as colorless crystals, identical with the compound from Example 33.

後処理

  1. customin the course of 5 minutes
  2. customrises from 25° to 35° C
  3. temperaturethe reaction mixture is then slowly raised to the boil
  4. temperatureIt is refluxed for 5 minutes
  5. filtrationfiltered hot
  6. concentrationthe filtrate is concentrated
  7. customAfter recrystallization from ethyl acetate/methanol

出典と根拠

ORDレコード
ord-76815d093611414aaacc6057aa4facfb
出典データセット
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04271163

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