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1-Hydroxybenzotriazole → HCID 14858896, 화합물

HRID 1074003
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HRID 1074003 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 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

생성물 1

HCID 14858896HCID 14858896, 화합물수율 102.9%

시약·촉매·용매

2
HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

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%)

후처리

  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

출처 및 근거

ORD 기록
ord-4eedc17f517e45229b4135d26a464a29
출처 데이터셋
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04971993

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