Triethylamine → HCID 178459241, 화합물

HRID 237336노트

반응식

HRID 237336 반응식
Cl.[Cl:2][C:3]1[CH:26]=[CH:25][C:6]2[N:7]3[C:11]([CH2:12][NH:13][CH2:14][C:5]=2[CH:4]=1)=[N:10][N:9]=[C:8]3[C@H:15]1[CH2:20][CH2:19][C@H:18]([O:21][CH:22]([CH3:24])[CH3:23])[CH2:17][CH2:16]1.C(N(CC)CC)C.[CH3:34][S:35](Cl)(=[O:37])=[O:36]>ClCCl>[Cl:2][C:3]1[CH:26]=[CH:25][C:6]2[N:7]3[C:11](=[N:10][N:9]=[C:8]3[C@H:15]3[CH2:16][CH2:17][C@H:18]([O:21][CH:22]([CH3:24])[CH3:23])[CH2:19][CH2:20]3)[CH2:12][N:13]([S:35]([CH3:34])(=[O:37])=[O:36])[CH2:14][C:5]=2[CH:4]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 178459238HCID 178459238, 화합물

생성물 1

HCID 178459241HCID 178459241, 화합물수율 5.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of trans-8-chloro-1-(4-isopropoxy-cyclohexyl)-5,6-dihydro-4H-2,3,5,10b-tetraaza-benzo[e]azulene hydrochloride (0.070 g, 0.18 mmol) and triethylamine (0.052 ml, 0.37 mmol) in dichloromethane (5 ml) was added methanesulfonyl chloride (0.015 ml, 0.19 mmol) at room temperature. After stirring for 19 h the reaction mixture was concentrated in vacuo. Flash-chromatography with n-heptane/2-propanol as eluent gave the title compound (0.004 g, 5%) as yellow solid. MS m/e: 439 (M+H+).

후처리

  1. concentrationwas concentrated in vacuo

출처 및 근거

ORD 기록
ord-296bb57f9d8345469ca470efb7a6d159
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08642590B2

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