Diisopropylethylamine → HCID 67902445, 화합물

HRID 232203노트

반응식

HRID 232203 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.C(N(C(C)C)CC)(C)C.Cl[C:28]1([C:34]([O:36][CH2:37][C:38]2[CH:43]=[CH:42][C:41]([N+:44]([O-:46])=[O:45])=[CH:40][CH:39]=2)=[O:35])[CH2:32][CH2:31][C:30](=[O:33])[O:29]1>ClCCl>[CH2:1]([O:8][C:9]([NH:11][C@@H:12]1[CH2:16][O:15][N:14]([C:28]2([C:34]([O:36][CH2:37][C:38]3[CH:43]=[CH:42][C:41]([N+:44]([O-:46])=[O:45])=[CH:40][CH:39]=3)=[O:35])[CH2:32][CH2:31][C:30](=[O:33])[O:29]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 81531DiisopropylethylamineHCID 14049831HCID 14049831, 화합물HCID 14181639HCID 14181639, 화합물

생성물 1

HCID 67902445HCID 67902445, 화합물수율 56%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 4 ml of dichloromethane was dissolved 60 mg of (4R)-4-benzyloxycarbonylamino-3-isoxazolidinone. To the solution were added under ice-cooling 0.08 ml of diisopropyl ethylamine and 90 mg of the Compound (15) obtained in Example 15. The mixture was stirred for 15 minutes under ice-cooling, followed by stirring at room temperature for 30 minutes. The reaction solution was washed with water, which was dried (Na2SO4), then the solvent was evaporated off. The residue was subjected to a silica gel column chromatography, followed by elution with hexane-ethyl acetate (1:1) to give 71 mg of the subject Compound (8) as colorless foamy product. The IR and NMR spectra of this product were in agreement with those of the Compound (8) obtained in Example 8.

후처리

  1. additionTo the solution were added under ice-
  2. temperaturecooling
  3. stirringby stirring at room temperature for 30 minutes
  4. washThe reaction solution was washed with water, which
  5. dry with materialwas dried (Na2SO4)
  6. customthe solvent was evaporated off
  7. washfollowed by elution with hexane-ethyl acetate (1:1)

출처 및 근거

ORD 기록
ord-3ac6b1211123457289d1d38d4b568b62
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851422

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