Triethylamine → HCID 178476475、化合物

HRID 237339ノート

反応式

HRID 237339 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.[C:34]([O:37][CH2:38][C:39](Cl)=[O:40])(=[O:36])[CH3:35]>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]([C:39](=[O:40])[CH2:38][O:37][C:34](=[O:36])[CH3:35])[CH2:14][C:5]=2[CH:4]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 26297Acetoxyacetyl chlorideHCID 178459238HCID 178459238、化合物

生成物 1

HCID 178476475HCID 178476475、化合物収率 70%

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 (0.090 g, 0.23 mmol) and triethylamine (0.066 ml, 0.48 mmol) in dichloromethane (5 ml) was added acetoxy acetyl chloride (0.031 g, 0.25 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 (0.073 g, 70%) as white solid. MS m/e: 461 (M+H+).

後処理

  1. concentrationwas concentrated in vacuo

出典と根拠

ORDレコード
ord-3b02779045da49dd82a817f68508b9e8
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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