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1-Hydroxybenzotriazole → HCID 14858896、化合物

HRID 1074003
ノート
印刷プレビュー

反応式

HRID 1074003 の反応式
C1(NC2CCCCC2)CCCCC1.[C:14]([O:18][C:19]([NH:21][C@H:22]([C:27]([OH:29])=O)[CH2:23][CH2:24][S:25][CH3:26])=[O:20])([CH3:17])([CH3:16])[CH3:15].Cl.[CH2:31]([O:38][C:39](=[O:45])[C@@H:40]1[CH2:44][CH2:43][CH2:42][NH:41]1)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl>C(Cl)Cl.CN(C)C=O>[CH2:31]([O:38][C:39](=[O:45])[C@@H:40]1[CH2:44][CH2:43][CH2:42][N:41]1[C:27](=[O:29])[C@H:22]([CH2:23][CH2:24][S:25][CH3:26])[NH:21][C:19]([O:18][C:14]([CH3:15])([CH3:16])[CH3:17])=[O:20])[C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 89856L-Methionine, N-[(1,1-dimethylethoxy)carbonyl]-, compd. with N-cyclohexylcyclohexanamine (1:1)HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 2733413Proline benzyl ester hydrochloride

生成物 1

HCID 14858896HCID 14858896、化合物収率 102.9%

試薬・触媒・溶媒

2
HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

N-t-butyloxycarbonyl-L-methionine dicyclohexylamine salt (44.36 g, 103 mmole), L-proline benzylester hydrochloride (2490 g, 103 mmole) and HOBT (13.92 g, 103 mmole) were dissolved in methylene chloride (400 ml), and WSC hydrochloride (19.75 g, 103 mmole) were added thereto at -30C. The mixture was stirred for 2 hours at less than 0° C., N,N-dimethylformamide (100 ml) was added thereto, and stirred further overnight at room temperature. The solution was washed with 5% aqueous sodium bicarbonate (400 ml, twice), 5% aqueous citric acid (400 ml, twice) and water (400 ml) in the order given, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain N-t-butyloxycarbonyl-L-methionyl-L-proline benzylester (yield: 46.27 g, 100%)

後処理

  1. stirringstirred further overnight at room temperature
  2. washThe solution was washed with 5% aqueous sodium bicarbonate (400 ml
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-4eedc17f517e45229b4135d26a464a29
出典データセット
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04971993

反応ノート

読み込み中…

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