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

Ethyl chloroacetate → 2-Benzylidenehydrazono-3-ethoxycarbonylmethyl-1-methoxycarbonylmethylimidazolidin-4-one

HRID 21408
ノート
印刷プレビュー

反応式

HRID 21408 の反応式
[H-].[Na+].[CH:3](=[N:10][N:11]=[C:12]1[NH:16][C:15](=[O:17])[CH2:14][N:13]1[CH2:18][C:19]([O:21][CH3:22])=[O:20])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26]>CN(C)C=O.C(Cl)(Cl)Cl.O>[CH:3](=[N:10][N:11]=[C:12]1[N:16]([CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])[C:15](=[O:17])[CH2:14][N:13]1[CH2:18][C:19]([O:21][CH3:22])=[O:20])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 1360406052-Benzylidenehydrazono-1-methoxycarbonylmethylimidazolidin-4-one

生成物 1

HCID 541207212-Benzylidenehydrazono-3-ethoxycarbonylmethyl-1-methoxycarbonylmethylimidazolidin-4-one収率 44.4%

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回
HCID 6212
Chloroform
溶媒
2 回
HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
30 °C

実験手順

In 20 ml of dimethylformamide (DMF) was suspended 96 mg of 60% sodium hydride under ice-cooling, 5 ml of a DMF solution of 548 mg of 2-benzylidenehydrazono-1-methoxycarbonylmethylimidazolidin-4-one was gradually added to the suspension. After stirring the mixture for one hour at 30° C., 254 mg of ethyl chloroacetate was gradually added dropwise thereto, followed by stirring for one hour at 80° C. After cooling the reaction mixture, water and chloroform was added thereto to distribute the mixture between water and chloroform, and the aqueous layer was further extracted three times with chloroform. The organic layer was combined with the extract, the mixture was dried over anhydrous magnesium sulfate, concentrated under reduced pressure, and the residue formed was recrystallized from a mixture of chloroform and n-hexane to obtain 320 mg of 2-benzylidenehydrazono-3-ethoxycarbonylmethyl-1-methoxycarbonylmethylimidazolidin-4-one.

後処理

  1. temperaturecooling
  2. stirringby stirring for one hour at 80° C
  3. additionwas added
  4. extractionthe aqueous layer was further extracted three times with chloroform
  5. dry with materialthe mixture was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customthe residue formed
  8. customwas recrystallized from a mixture of chloroform and n-hexane

出典と根拠

ORDレコード
ord-95f5bb33bf7440c88b09193ba4fb2a51
出典データセット
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05422360

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート