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

HRID 1380186노트

반응식

HRID 1380186 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  1. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-811a1a7e3630480fad8b701ec1191062
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579947

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