Dichloromethane → 1-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-(4-ethoxycarbonylphenyl)urea hydrochloride

HRID 543173

反応式

HRID 543173 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.C(N(CC)CC)C.[CH2:32]([O:34][C:35]([C:37]1[CH:42]=[CH:41][C:40]([N:43]=[C:44]=[O:45])=[CH:39][CH:38]=1)=[O:36])[CH3:33]>O1CCCC1>[ClH:21].[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:44]([NH:43][C:40]3[CH:39]=[CH:38][C:37]([C:35]([O:34][CH2:32][CH3:33])=[O:36])=[CH:42][CH:41]=3)=[O:45])[CH2:9][CH2:10]2)=[CH:20][CH:19]=1

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 589805Ethyl 4-isocyanatobenzoateHCID 202057391-(3-Aminopropyl)-4-(4-chlorobenzyl)piperazine trihydrochloride

生成物 1

HCID 202057461-{3-[4-(4-Chlorobenzyl)piperazin-1-yl]propyl}-3-(4-ethoxycarbonylphenyl)urea hydrochloride収率 62.8%

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 (7.54 g; 20 mmole), methylene chloride (50 ml), tetrahydrofuran (50 ml), triethylamine (8.4 ml; 60 mmole) and 4-ethoxycarbonylphenyl isocyanate (3.8 g; 20 mmole). Recrystallization from methanol provided the title compound (3.11 g; 34% yield) as colorless crystals, m.p. 233°-234° C.

後処理

  1. customRecrystallization from methanol

出典と根拠

ORDレコード
ord-6f06b869d3c54d2fb05d7bf41d832f2f
出典データセット
uspto-grants-1987_04
特許番号
US04661481

関連ノート

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