HCID 14300313, 화합물 → A85 4777

HRID 1761847노트

반응식

HRID 1761847 반응식
[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]

참가 물질

5

반응물 2

HCID 14300313HCID 14300313, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 3082813A85 4777

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f4b465d208cf495fbee4a2f9bf89f768
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04829061

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