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tert-Butyl 4-(methylamino)piperidine-1-carboxylate → tert-butyl 4-({-[(E)-2-(4'-chlorobiphenyl-4-ylcarbamoyl)vinyl]benzyl}methylamino)piperidine-1-carboxylate

HRID 735178
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인쇄 미리보기

반응식

HRID 735178 반응식
C[NH:2][CH:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]1.[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[CH:28]=[CH:27][C:26]([NH:29][C:30](=[O:41])/[CH:31]=[CH:32]/[C:33]3[CH:38]=CC(CCl)=[CH:35][CH:34]=3)=[CH:25][CH:24]=2)=[CH:19][CH:18]=1>CN(C=O)C>[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[CH:24]=[CH:25][C:26]([NH:29][C:30](/[CH:31]=[CH:32]/[CH:33]([CH2:38][NH:2][CH:3]3[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]3)[C:34]3[CH:5]=[CH:4][CH:3]=[CH:8][CH:35]=3)=[O:41])=[CH:27][CH:28]=2)=[CH:19][CH:18]=1
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참가 물질

4

반응물 2

HCID 15380702tert-Butyl 4-(methylamino)piperidine-1-carboxylateHCID 68816418(E)-N-(4'-chlorobiphenyl-4-yl)-3-(4-chloromethylphenyl)acrylamide

생성물 1

HCID 86601894tert-butyl 4-({-[(E)-2-(4'-chlorobiphenyl-4-ylcarbamoyl)vinyl]benzyl}methylamino)piperidine-1-carboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
80 °C

실험 절차

0.5 g (2.34 mmol) of tert-butyl 4-methylaminopiperidine-1-carboxylate is added to a suspension of 300 mg (0.79 mmol) of (E)-N-(4′-chlorobiphenyl-4-yl)-3-(4-chloromethylphenyl)acrylamide in 5 mL of DMF and the mixture is stirred for 18 hours at 80° C. Then the reaction mixture is poured onto water and the precipitate formed is suction filtered. Further purification is carried out by stirring out from a little methanol. Yield: 200 mg (45% of theory); C33H38ClN3O3 (M=560.13); melting point: 168° C.-169° C.; calc.: molecular ion peak (M+H)+: 560/562 (Cl); found: molecular ion peak (M+H)+: 560/562 (Cl).

후처리

  1. additionThen the reaction mixture is poured onto water
  2. customthe precipitate formed
  3. filtrationfiltered
  4. customFurther purification
  5. stirringby stirring out from a little methanol

출처 및 근거

ORD 기록
ord-967537c06e3c41b19274ab1e13016194
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07592373B2

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