Triethylamine → HCID 67902483、化合物

HRID 232232ノート

反応式

HRID 232232 の反応式
[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

参加物

5

反応物 3

HCID 8471TriethylamineHCID 14181640HCID 14181640、化合物HCID 20030930HCID 20030930、化合物

生成物 1

HCID 67902483HCID 67902483、化合物収率 64.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-70a207bade0a42bea2dbf24e17429536
出典データセット
uspto-grants-1989_07
特許番号
US04851422

反応ノート

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