Triethylamine → HCID 178459241、化合物

HRID 237336ノート

反応式

HRID 237336 の反応式
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

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 178459238HCID 178459238、化合物

生成物 1

HCID 178459241HCID 178459241、化合物収率 5.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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+).

後処理

  1. concentrationwas concentrated in vacuo

出典と根拠

ORDレコード
ord-296bb57f9d8345469ca470efb7a6d159
出典データセット
uspto-grants-2014_02
特許番号
US08642590B2

反応ノート

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