Propyl isocyanate → 4-[2-[4-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-yl)-1-piperazinyl]-2-oxoethyl]-N-propyl-1-piperidinecarboxamide

HRID 47351

反応式

HRID 47351 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[CH2:12][CH2:11][C:10]3[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:9]=3[CH:8]([N:18]3[CH2:23][CH2:22][N:21]([C:24](=[O:32])[CH2:25][CH:26]4[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]4)[CH2:20][CH2:19]3)[C:5]2=[N:6][CH:7]=1.[CH2:33]([N:36]=[C:37]=[O:38])[CH2:34][CH3:35]>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]2[CH2:12][CH2:11][C:10]3[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:9]=3[CH:8]([N:18]3[CH2:19][CH2:20][N:21]([C:24](=[O:32])[CH2:25][CH:26]4[CH2:31][CH2:30][N:29]([C:37]([NH:36][CH2:33][CH2:34][CH3:35])=[O:38])[CH2:28][CH2:27]4)[CH2:22][CH2:23]3)[C:5]2=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 61033Propyl isocyanateHCID 107682201-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-yl)-4-[(4-piperidinyl)acetyl]piperazine

生成物 1

HCID 107699304-[2-[4-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-yl)-1-piperazinyl]-2-oxoethyl]-N-propyl-1-piperidinecarboxamide収率 112.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

1-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-yl)-4-[(4-piperidinyl)acetyl]piperazine (Preparative Example 10) (490 mg, 0.8 mmoles) was dissolved in anhydrous dichloromethane (5 ml) and n-propyl isocyanate (322.1 mg, 3.2 mmoles) was added. The mixture was stirred under argon at 25° C. for 44 h. The solution was chromatographed on silica gel using 2% (10% concentrated NH4OH in methanol)dichloromethane as the eluant to give 544.8 mg of the title compound (Yield: 95%).

後処理

  1. customThe solution was chromatographed on silica gel using 2% (10% concentrated NH4OH in methanol)dichloromethane as the eluant

出典と根拠

ORDレコード
ord-1951beaeb4f14e549384a1c72b7a7480
出典データセット
uspto-grants-2004_03
特許番号
US06699872B2

関連ノート

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