Triethylamine → 1-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-(4-cyanophenyl)urea dihydrochloride monohydrate

HRID 1380196

反応式

HRID 1380196 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]=[C:10]=[O:11])=[CH:5][CH:4]=1)#[N:2].[ClH:12].Cl.Cl.[NH2:15][CH2:16][CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][N:22]([CH2:25][C:26]2[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][CH:27]=2)[CH2:21][CH2:20]1.C(N(CC)CC)C>C(Cl)Cl>[OH2:11].[ClH:32].[ClH:12].[Cl:32][C:29]1[CH:30]=[CH:31][C:26]([CH2:25][N:22]2[CH2:21][CH2:20][N:19]([CH2:18][CH2:17][CH2:16][NH:15][C:10]([NH:9][C:6]3[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:8][CH:7]=3)=[O:11])[CH2:24][CH2:23]2)=[CH:27][CH:28]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 1703804-Cyanophenyl isocyanateHCID 202057391-(3-Aminopropyl)-4-(4-chlorobenzyl)piperazine trihydrochloride

生成物 1

HCID 202057271-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-(4-cyanophenyl)urea dihydrochloride monohydrate収率 153.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The procedure described in Example 21 was followed, using 4-cyanophenyl isocyanate (1.44 g; 10 mmole), 1-(3-aminopropyl)-4-(4-chlorobenzyl)piperazine trihydrochloride (3.77 g; 10 mmole), methylene chloride (75 ml) and triethylamine (4.3 ml; 31 mmole). Recrystallization from methanol/ethanol provided the title compound (3.87 g; 77% yield) as colorless crystals, m.p. 236°-238° C.

後処理

  1. customRecrystallization from methanol/ethanol

出典と根拠

ORDレコード
ord-071890b6ec2040e6936d3e46db8bd75d
出典データセット
uspto-grants-1986_04
特許番号
US04579947

関連ノート

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