Triethylamine → HCID 15927688, 화합물

HRID 330623노트

반응식

HRID 330623 반응식
Br[CH:2]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][N:15]1[C:19](=[O:20])[C:18]2=[CH:21][CH:22]=[CH:23][CH:24]=[C:17]2[C:16]1=[O:25])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[C:26]([O:30][C:31](=[O:42])[C@@H:32]1[CH2:36][CH2:35][CH2:34][N:33]1[C:37](=[O:41])[C@H:38]([CH3:40])[NH2:39])([CH3:29])([CH3:28])[CH3:27].C(N(CC)CC)C>C(#N)C>[C:26]([O:30][C:31](=[O:42])[C@@H:32]1[CH2:36][CH2:35][CH2:34][N:33]1[C:37](=[O:41])[C@H:38]([CH3:40])[NH:39][C@@H:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][N:15]1[C:19](=[O:20])[C:18]2=[CH:21][CH:22]=[CH:23][CH:24]=[C:17]2[C:16]1=[O:25])([CH3:28])([CH3:27])[CH3:29]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12939800tert-Butyl L-alanyl-L-prolinateHCID 13622534Ethyl 2-bromo-9-phthalimidononanoate

생성물 1

HCID 15927688HCID 15927688, 화합물수율 13.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of ethyl 2-bromo-9-phthalimidononanoate [prepared according to Chem. Pharm. Bull. 34, 2078 (1986)] (3 g), L-alanyl-L-proline tertiary butylester (1 g) and triethylamine (0.8 ml) in acetonitrile (200 ml) is subjected to 60 hours' reflux. Acetonitrile is distilled off under reduced pressure, and the residue is dissolved in ethyl acetate. The solution is dehydrated with anhydrous sodium sulfate, and thereafter is concentrated to obtain an oily residue. When this substance is applied to a silica gel chromatography (ethyl acetate:n-hexane=3:1) for separative purification, 310 mg of N-[1(R)-ethoxycarbonyl-8-phthalimidooctyl]-L-alanyl-L-proline tertiary butylester is obtained as a colorless oil from the first effluence.

후처리

  1. temperature' reflux
  2. distillationAcetonitrile is distilled off under reduced pressure
  3. dissolutionthe residue is dissolved in ethyl acetate
  4. concentrationis concentrated
  5. customto obtain an oily residue
  6. customWhen this substance is applied to a silica gel chromatography (ethyl acetate:n-hexane=3:1) for separative purification

출처 및 근거

ORD 기록
ord-634fc89166d84c45b81d6c9f9789ba58
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04897483

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