HCID 14300313，化合物 → 化合物 T26457

HRID 1761847笔记

反应方程式

HRID 1761847 反应方程式
[OH:1][C:2]1[C:26]([C:27]([CH3:30])([CH3:29])[CH3:28])=[CH:25][C:5]([C:6]([N:8]2[CH2:14][CH2:13][CH2:12][N:11](C(OCC3C=CC=CC=3)=O)[CH2:10][CH2:9]2)=[O:7])=[CH:4][C:3]=1[C:31]([CH3:34])([CH3:33])[CH3:32].[H][H]>[Pd].C(O)(=O)C>[OH:1][C:2]1[C:3]([C:31]([CH3:33])([CH3:32])[CH3:34])=[CH:4][C:5]([C:6]([N:8]2[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[O:7])=[CH:25][C:26]=1[C:27]([CH3:30])([CH3:29])[CH3:28]

参与物

5

反应物 2

HCID 14300313HCID 14300313，化合物HCID 178418361HCID 178418361，化合物

产物 1

HCID 3082813化合物 T26457

试剂、催化剂与溶剂 2

HCID 23938钯碳催化剂HCID 176醋酸溶剂

实验过程

A mixture of 46.6 g (0.1 mol) of 1-(4-hydroxy-3,5-di-tert.-butylbenzoyl)-4-benzyloxycarbonylhomopiperazine (Example 1), 350 ml of glacial acetic acid and 2.3 g of palladium black is treated with hydrogen while stirring at 70°-80° C. for about 7 hours. The catalyst is then filtered off, and the solvent is removed by distillation under reduced pressure. The residue is dissolved in methylene chloride, and the solution is extracted by shaking with dilute sodium hydroxide solution and separated off. The organic phase is washed several times with water and then dried over anhydrous sodium sulfate. The residue left after the solvent has been removed in vacuo is recrystallized from acetonitrile with the addition of active charcoal.

后处理

  1. filtrationThe catalyst is then filtered off
  2. customthe solvent is removed by distillation under reduced pressure
  3. dissolutionThe residue is dissolved in methylene chloride
  4. extractionthe solution is extracted
  5. stirringby shaking with dilute sodium hydroxide solution
  6. customseparated off
  7. washThe organic phase is washed several times with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. waitThe residue left after the solvent
  10. customhas been removed in vacuo
  11. customis recrystallized from acetonitrile with the addition of active charcoal

来源与证据

ORD记录
ord-f4b465d208cf495fbee4a2f9bf89f768
来源数据集
uspto-grants-1989_05
专利号
US04829061

反应笔记

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