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4-Piperidineethanol → HCID 68303884, 화합물

HRID 1846613
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인쇄 미리보기

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HRID 1846613 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:16]=[CH:17][CH:18]=1)[C:5]([NH:7][C:8]1[C:9](Cl)=[N:10][CH:11]=[C:12]([Cl:14])[CH:13]=1)=[O:6].[NH:19]1[CH2:24][CH2:23][CH:22]([CH2:25][CH2:26][OH:27])[CH2:21][CH2:20]1>C(#N)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:16]=[CH:17][CH:18]=1)[C:5]([NH:7][C:8]1[C:9]([N:19]2[CH2:24][CH2:23][CH:22]([CH2:25][CH2:26][OH:27])[CH2:21][CH2:20]2)=[N:10][CH:11]=[C:12]([Cl:14])[CH:13]=1)=[O:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 739534-PiperidineethanolHCID 86676282HCID 86676282, 화합물

생성물 1

HCID 68303884HCID 68303884, 화합물수율 99.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
180 °C

실험 절차

A mixture of 1.06 g (5.00 mmol) of 3-chloro-N-(2,5-dichloro-pyridin-3-yl)-benzamide and 0.646 g (5.00 mmol) of 4-piperidine ethanol in acetonitrile (25 mL) is heated in a microwave reactor at 180° C. for 4 hours. Upon standing at room temperature a solid precipitates from solution. The solid is collected by filtration, washed with cold acetonitrile, and dried on the filter pad to provide 1.97 g (76%) of 3-chloro-N-[5′-chloro-4-(2-hydroxy-ethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-3′-yl]-benzamide as a clear solid.

후처리

  1. customUpon standing at room temperature
  2. customprecipitates from solution
  3. filtrationThe solid is collected by filtration
  4. washwashed with cold acetonitrile
  5. customdried on the filter pad

출처 및 근거

ORD 기록
ord-e67c5fb5e17b429e8f332e199156cba2
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952004B2

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