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

HRID 1267987
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반응식

HRID 1267987 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
참가 물질실험 절차후처리출처 및 근거반응 노트

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), (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-ad555c4af99942f1a70d19c5bd62b9a9
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06555537B2

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