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4-Chlorobenzylpiperazine → 1-(((4-Chlorobenzyl)amino)carbonyl)-4-(4-chlorobenzyl)piperazine

HRID 1368209
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반응식

HRID 1368209 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]([CH2:6][N:7]=[C:8]=[O:9])=[CH:4][CH:3]=1.[Cl:12][C:13]1[CH:25]=[CH:24][C:16]([CH2:17][N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[CH:15][CH:14]=1>C1COCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][NH:7][C:8]([N:21]2[CH2:20][CH2:19][N:18]([CH2:17][C:16]3[CH:24]=[CH:25][C:13]([Cl:12])=[CH:14][CH:15]=3)[CH2:23][CH2:22]2)=[O:9])=[CH:10][CH:11]=1
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참가 물질

4

반응물 2

HCID 1348264-ChlorobenzylpiperazineHCID 33723791-Chloro-4-(isocyanatomethyl)benzene

생성물 1

HCID 222649801-(((4-Chlorobenzyl)amino)carbonyl)-4-(4-chlorobenzyl)piperazine수율 54.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4-chlorobenzylisocyanate (0.59 g, 3.5 mmol) in anhydrous THF (15 mL) at 0° C. was added 1-(4-chlorobenzyl)piperazine (0.74 g, 3.5 mmol). The resultant mixture was stirred at ambient temperature. After 20 hours the mixture was concentrated of volatiles. The resulting solid was washed with ethyl acetate and dried in vacuo to afford 0.72 g of 1-(((4-chlorobenzyl)amino)carbonyl)-4-(4-chlorobenzyl)piperazine as a white solid; NMR (CDCl3) 7.4 (m, 4), 7.3 (m, 2), 7.2 (m, 2), 4.4-4.1 (m, 6), 3.6 (m, 4), 3.0 (m, 2) ppm.

후처리

  1. concentrationAfter 20 hours the mixture was concentrated of volatiles
  2. washThe resulting solid was washed with ethyl acetate
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-e14ae20502594e2a836253c1ef215c16
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06573266B1

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