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

HRID 543175

反応式

HRID 543175 の反応式
Cl.Cl.Cl.[NH2:4][CH2:5][CH2:6][CH2:7][N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1.C(Cl)[Cl:23].C(N(CC)CC)C.[F:32][C:33]1[CH:38]=[CH:37][C:36]([N:39]=[C:40]=[O:41])=[CH:35][CH:34]=1>O1CCCC1>[OH2:41].[ClH:21].[ClH:23].[Cl:21][C:18]1[CH:17]=[CH:16][C:15]([CH2:14][N:11]2[CH2:12][CH2:13][N:8]([CH2:7][CH2:6][CH2:5][NH:4][C:40]([NH:39][C:36]3[CH:37]=[CH:38][C:33]([F:32])=[CH:34][CH:35]=3)=[O:41])[CH2:9][CH2:10]2)=[CH:20][CH:19]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 709554-Fluorophenyl isocyanateHCID 202057391-(3-Aminopropyl)-4-(4-chlorobenzyl)piperazine trihydrochloride

生成物 1

HCID 202057601-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-(4-fluorophenyl)urea dihydrochloride monohydrate収率 76%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The procedure described in Example 3 was followed, using 1-(3-aminopropyl)-4-(4-chlorobenzyl)piperazine trihydrochloride (3.77 g; 10 mmole), methylene chloride (50 ml), tetrahydrofuran (10 ml), triethylamine (4.2 ml; 30 mmole) and 4-fluorophenyl isocyanate (1.37 g; 10 mmole). Recrystallization from methanol/methylene chloride provided the title compound (3.75 g; 76% yield) as colorless crystals, m.p. 225°-228° C.

後処理

  1. customRecrystallization from methanol/methylene chloride

出典と根拠

ORDレコード
ord-55c018c5b4404a72a5e386e750468415
出典データセット
uspto-grants-1987_04
特許番号
US04661481

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