Triethylamine → HCID 67902483, 화합물

HRID 232232노트

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HRID 232232 반응식
[CH2:1]([O:8][C:9]([NH:11][C@H:12]1[CH2:16][O:15][NH:14][C:13]1=[O:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:19]1([C:29]([O:31][CH2:32][C:33]2[CH:38]=[CH:37][C:36]([N+:39]([O-:41])=[O:40])=[CH:35][CH:34]=2)=[O:30])[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:21](=[O:28])[O:20]1.C(N(CC)CC)C>ClCCl>[CH2:1]([O:8][C:9]([NH:11][C@H:12]1[CH2:16][O:15][N:14]([C:19]2([C:29]([O:31][CH2:32][C:33]3[CH:38]=[CH:37][C:36]([N+:39]([O-:41])=[O:40])=[CH:35][CH:34]=3)=[O:30])[C:27]3[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=3)[C:21](=[O:28])[O:20]2)[C:13]1=[O:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 14181640HCID 14181640, 화합물HCID 20030930HCID 20030930, 화합물

생성물 1

HCID 67902483HCID 67902483, 화합물수율 64.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 5 ml of dichloromethane were dissolved 236 mg of (4S)-4-benzyloxycarbonylamino-3-isoxazolidinone and 347 mg of Compound (98). To the solution was added, under ice-cooling, 0.14 ml of triethylamine, and the mixture was stirred for 30 minutes. The solvent was evaporated off. To the residue was added ethyl acetate, which was washed with water and an aqueous saline solution. The organic layer was dried, then the solvent was evaporated off. The residue was subjected to a column chromatography using Florisil, followed by elution with hexane--ethyl acetate (2:1→1:1) to give 350 mg of the subject Compound (99) as a pale yellow oily product.

후처리

  1. additionTo the solution was added, under ice-
  2. temperaturecooling
  3. customThe solvent was evaporated off
  4. additionTo the residue was added ethyl acetate, which
  5. washwas washed with water
  6. customThe organic layer was dried
  7. customthe solvent was evaporated off
  8. washfollowed by elution with hexane--ethyl acetate (2:1→1:1)

출처 및 근거

ORD 기록
ord-70a207bade0a42bea2dbf24e17429536
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851422

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