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Diethyl Ether → HCID 86655277, 화합물

HRID 2192339
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HRID 2192339 반응식
[Cl:1][CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)=[O:4].[N:12]12[CH2:19][CH2:18][CH:15]([CH2:16][CH2:17]1)[C@@H:14]([O:20][C:21]([C:23]1([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]1)=[O:22])[CH2:13]2.C(OCC)C>C(#N)C>[Cl-:1].[C:30]1([C:23]2([C:21]([O:20][C@@H:14]3[CH:15]4[CH2:18][CH2:19][N+:12]([CH2:2][C:3](=[O:4])[NH:5][C:6]5[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=5)([CH2:17][CH2:16]4)[CH2:13]3)=[O:22])[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]2)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 43824892-chloro-N-(pyridin-4-yl)acetamideHCID 591796191-Phenyl-cycloheptanecarboxylic acid (R)-(1-aza-bicyclo[2.2.2]oct-3-yl)ester

생성물 1

HCID 86655277HCID 86655277, 화합물수율 24.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

2-Chloro-N-pyridin-4-yl-acetamide (Example 16a) (30 mg) was added to a solution of 1-phenyl-cycloheptanecarboxylic acid (R)-(1-aza-bicyclo[2.2.2]oct-3-yl)ester (Example 14e) (53 mg) in acetonitrile (1 mL). The reaction mixture was stirred at room temperature for 24 h. Diethyl ether (2 mL) was added and the reaction mixture was filtered to give a light brown solid. The solid was washed several times with diethyl ether and dried under vacuum at 40° C. Purification by column chromatography eluting with 0-10% MeOH/ dichloromethane gave the title compound as a white solid (20 mg).

후처리

  1. filtrationthe reaction mixture was filtered
  2. customto give a light brown solid
  3. washThe solid was washed several times with diethyl ether
  4. customdried under vacuum at 40° C
  5. customPurification by column chromatography
  6. washeluting with 0-10% MeOH/ dichloromethane

출처 및 근거

ORD 기록
ord-f230f70bf7cf402590b9c1dc0a7d7dd5
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08329729B2

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