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

HRID 1761846노트

반응식

HRID 1761846 반응식
[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]

참가 물질

4

반응물 2

HCID 37871873,5-Di-tert-butyl-4-hydroxybenzoyl chlorideHCID 4384955Benzyl 1,4-diazepane-1-carboxylate

생성물 1

HCID 14300313HCID 14300313, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-adf67d0c2e6d4c239ebb395b912a1ae6
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04829061

반응 노트

불러오는 중…