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3-Aminobenzonitrile → trans-3-(3-Bromo-phenyl)-4-(3-cyano-phenylcarbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester

HRID 1524288
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HRID 1524288 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:12][C@@H:11]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Br:19])[CH:14]=2)[C@H:10]([C:20](O)=[O:21])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:23][C:24]1[CH:25]=[C:26]([CH:29]=[CH:30][CH:31]=1)[C:27]#[N:28].P(Cl)(Cl)(Cl)=O>N1C=CC=CC=1.O>[C:1]([O:5][C:6]([N:8]1[CH2:9][C@@H:10]([C:20](=[O:21])[NH:23][C:24]2[CH:31]=[CH:30][CH:29]=[C:26]([C:27]#[N:28])[CH:25]=2)[C@H:11]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Br:19])[CH:14]=2)[CH2:12]1)=[O:7])([CH3:3])([CH3:4])[CH3:2]
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참가 물질

6

반응물 3

HCID 167023-AminobenzonitrileHCID 24813Phosphorus oxychlorideHCID 2762118Trans-4-(3-bromophenyl)-1-Boc-pyrrolidine-3-carboxylic acid

생성물 1

HCID 68089325trans-3-(3-Bromo-phenyl)-4-(3-cyano-phenylcarbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester수율 83.5%

시약·촉매·용매 2

HCID 962Water용매
HCID 1049
Pyridine
용매

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온도
0 °C

실험 절차

Cool a solution of trans-4-(3-bromo-phenyl)-pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester (0.50 g, 1.35 mmol) in pyridine (5 mL), to 0° C., and add 3-aminobenzonitrile (0.18 g, 1.48 mmol) followed by phosphorous oxychloride (0.14 mL, 1.50 mmol). Stir the mixture at 0° C. for 1 h then dilute with water. Extract the mixture with EtOAc and wash the combined organic portion with a 2 N solution of hydrochloric acid until the pH of the aqueous washings is strongly acidic. Wash the organic phase with brine then dry over anhydrous sodium sulfate and concentrate under reduced pressure. Purify the residue by flash silica gel chromatography to provide 0.53 g of trans-3-(3-bromo-phenyl)-4-(3-cyano-phenylcarbamoyl)-pyrrolidine-1-carboxylic acid tert-butyl ester as a solid.

후처리

  1. extractionExtract the mixture with EtOAc
  2. washwash the combined organic portion with a 2 N solution of hydrochloric acid until the pH of the aqueous washings
  3. washWash the organic phase with brine
  4. dry with materialthen dry over anhydrous sodium sulfate
  5. concentrationconcentrate under reduced pressure
  6. customPurify the residue by flash silica gel chromatography

출처 및 근거

ORD 기록
ord-8588fe25c8d84a39abb4408f90e4ab2e
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09079880B2

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