Triethylamine → HCID 53662264, 화합물

HRID 1720323노트

반응식

HRID 1720323 반응식
[CH2:1]([O:3][C:4]([CH:6]1[CH:18]([CH2:19][O:20][CH3:21])[C:17]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][C:15]=3[CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[Cl:29])[NH:10][C:9]=2[CH2:8][NH:7]1)=[O:5])[CH3:2].C(N(CC)CC)C.C(OCl)(C)(C)C>C1(C)C=CC=CC=1.ClCCl>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18]=1[CH2:19][O:20][CH3:21])=[C:15]([CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[Cl:29])[CH:14]=[CH:13][CH:12]=3)=[O:5])[CH3:2]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 521297Tert-Butyl hypochloriteHCID 545410741,2,3,4-Tetrahydro-5-(2-chlorobenzyl)-4-methoxymethyl-beta-carboline-3-carboxylic acid ethyl ester

생성물 1

HCID 53662264HCID 53662264, 화합물수율 33.6%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매2회

실험 절차

1 g (0.0024 mol) of 1,2,3,4-tetrahydro-5-(2-chlorobenzyl)-4-methoxymethyl-β-carboline-3-carboxylic acid ethyl ester is mixed in a mixture of 20 ml of toluene and 7 ml of dichloromethane at -15° C. with 1.2 ml of triethylamine. Then 0.9 ml (0.0074 mol) of tert.butylhypochlorite, dissolved in 12 ml of dichloromethane, is instilled. The reaction mixture is stirred at room temperature for two more hours. The evaporation residue is chromatographed on silica gel with equal parts of acetone and dichloromethane and yields 0.33 g (33% of theory) of 5-(2-chlorobenzyl)-4-methoxymethyl-β-carboline-3-carboxylic acid ethyl ester, melting point 182°-184° C. (from ethanol).

후처리

  1. customThe evaporation residue is chromatographed on silica gel with equal parts of acetone and dichloromethane

출처 및 근거

ORD 기록
ord-3332e4d99bd34a488c8ca6e37219bbb0
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05506234

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