Triethylamine → HCID 67902341, 화합물

HRID 232216노트

반응식

HRID 232216 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(CC)CC)C.Cl[C:26]1([C:38]([O:40][CH2:41][C:42]2[CH:47]=[CH:46][C:45]([N+:48]([O-:50])=[O:49])=[CH:44][CH:43]=2)=[O:39])[CH2:30][CH:29]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:28](=[O:37])[O:27]1>ClCCl>[CH2:1]([O:8][C:9]([NH:11][C@H:12]1[CH2:16][O:15][N:14]([C:26]2([C:38]([O:40][CH2:41][C:42]3[CH:43]=[CH:44][C:45]([N+:48]([O-:50])=[O:49])=[CH:46][CH:47]=3)=[O:39])[CH2:30][CH:29]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[C:28](=[O:37])[O:27]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 20030906HCID 20030906, 화합물

생성물 1

HCID 67902341HCID 67902341, 화합물수율 68.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Production of Compound(64): In 6 ml of dichloromethane was suspended 280 mg of (4S)-4-benzyloxycarbonylamino-3-isoxazolidinone. To the suspension were added, under ice-cooling and stirring, 0.36 ml of triethylamine and 490 mg of the Compound (63) obtained in Example 63 dissolved in 1 ml of dichloromethane. The reaction was solution stirred at room temperature for 30 minutes, which was washed with water and dried (MgSO4). The solvent was evaporated off, and the residue was chromatographed on silica gel, followed by elution with hexane-ethylacetate (3:1) to give 470 mg of the subject Compound (64) as colorless oily product. The IR and NMR spectra of this product were in agreement with those of the Compound (64) obtained in Example 64.

후처리

  1. additionTo the suspension were added, under ice-
  2. temperaturecooling
  3. stirringstirred at room temperature for 30 minutes
  4. washwhich was washed with water
  5. dry with materialdried (MgSO4)
  6. customThe solvent was evaporated off
  7. customthe residue was chromatographed on silica gel
  8. washfollowed by elution with hexane-ethylacetate (3:1)

출처 및 근거

ORD 기록
ord-802f197d391741119935f4f88e58b2ac
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851422

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