Sodium hydride → HCID 67693623、化合物

HRID 1417307

反応式

HRID 1417307 の反応式
[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.[H-].[Na+].[Na].Cl[CH2:17]/[CH:18]=[CH:19]/[CH2:20][N:21]1[C:29](=[O:30])[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:22]1=[O:31]>CN(C)C=O>[N:1]1([C:6]2[CH:11]=[CH:10][C:9]([O:12][CH2:17]/[CH:18]=[CH:19]/[CH2:20][N:21]3[C:29](=[O:30])[C:28]4[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=4)[C:22]3=[O:31])=[CH:8][CH:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

参加物

6

反応物 4

HCID 24758Sodium hydrideHCID 823151-(p-Hydroxyphenyl)imidazoleHCID 5360545SodiumHCID 57093742-((2E)-4-chlorobut-2-en-1-yl)-2,3-dihydro-1H-isoindole-1,3-dione

生成物 1

HCID 67693623HCID 67693623、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 16.0 g of 4-(1H-imidazol-1-yl)phenol in 250 ml of dimethylformamide, is treated with 4.2 g of 60% NaH. To the suspension of the sodium salt, 23.5 g of (E)-2-[4-chloro-2-buten-1-yl)-1H-isoindole-1,3(2H)-dione is added, and the reaction mixture stirred and heated on the steam bath for 16 hours. The dimethylformamide is removed in vacuo, and the residue stirred with 250 ml of water. The insolubles are collected, washed with water, and dried. Recrystallization from ethanol gives the desired product as a solid, m.p. 170°-171° C.

後処理

  1. additionis added
  2. temperatureheated on the steam bath for 16 hours
  3. customThe dimethylformamide is removed in vacuo
  4. stirringthe residue stirred with 250 ml of water
  5. customThe insolubles are collected
  6. washwashed with water
  7. customdried
  8. customRecrystallization from ethanol

出典と根拠

ORDレコード
ord-7e2c0457e8cc4b2d85de1791618a8f7c
出典データセット
uspto-grants-1999_03
特許番号
US05877196

関連ノート

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