Triethylamine → HCID 15927688、化合物

HRID 330623

反応式

HRID 330623 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 15927688HCID 15927688、化合物収率 13.1%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-634fc89166d84c45b81d6c9f9789ba58
出典データセット
uspto-grants-1990_01
特許番号
US04897483

関連ノート

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