3,5-Di-tert-butyl-4-hydroxybenzoyl chloride → HCID 14300313，化合物

HRID 1761846笔记

反应方程式

HRID 1761846 反应方程式
[C:1]([C:5]1[CH:6]=[C:7]([CH:11]=[C:12]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:13]=1[OH:14])[C:8](Cl)=[O:9])([CH3:4])([CH3:3])[CH3:2].[CH2:19]([O:26][C:27]([N:29]1[CH2:35][CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1)=[O:28])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C(#N)C>[OH:14][C:13]1[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:6][C:7]([C:8]([N:32]2[CH2:33][CH2:34][CH2:35][N:29]([C:27]([O:26][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[O:28])[CH2:30][CH2:31]2)=[O:9])=[CH:11][C:12]=1[C:15]([CH3:18])([CH3:17])[CH3:16]

参与物

4

反应物 2

HCID 37871873,5-Di-tert-butyl-4-hydroxybenzoyl chlorideHCID 43849551-高哌嗪羧酸苄酯

产物 1

HCID 14300313HCID 14300313，化合物

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

实验过程

A mixture of 13.4 g (0.05 mol) of 3,5-di-tert.-butyl-4-hydroxybenzoyl chloride and 12.4 g (0.053 mol) of 1-benzyloxycarbonylhomopiperazine in 200 ml of acetonitrile is heated under reflux, with stirring, for 6 hour. The solvent is then removed by distillation under reduced pressure, the residue is partitioned between methylene chloride and dilute hydrochloric acid, and the organic phase is separated off and washed with saturated brine. After drying over sodium sulfate and removal of the solvent by distillation under reduced pressure, the crystalline residue is digested with hot diisopropyl ether, filtered off with suction, washed with diisopropyl ether and dried.

后处理

  1. temperatureis heated
  2. temperatureunder reflux
  3. customThe solvent is then removed by distillation under reduced pressure
  4. customthe residue is partitioned between methylene chloride and dilute hydrochloric acid
  5. customthe organic phase is separated off
  6. washwashed with saturated brine
  7. dry with materialAfter drying over sodium sulfate and removal of the solvent by distillation under reduced pressure
  8. filtrationfiltered off with suction
  9. washwashed with diisopropyl ether
  10. customdried

来源与证据

ORD记录
ord-adf67d0c2e6d4c239ebb395b912a1ae6
来源数据集
uspto-grants-1989_05
专利号
US04829061

反应笔记

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