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Phosphorus oxychloride → 7-Chloro-2-phenylthieno[3,2-b]pyridine-6-carbonitrile

HRID 1611501
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반응식

HRID 1611501 반응식
O=[C:2]1[C:7]([C:8]#[N:9])=[CH:6][NH:5][C:4]2[CH:10]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[S:12][C:3]1=2.P(Cl)(Cl)([Cl:21])=O>CCCCCC>[Cl:21][C:2]1[C:7]([C:8]#[N:9])=[CH:6][N:5]=[C:4]2[CH:10]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[S:12][C:3]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 222566677-Oxo-2-phenyl-4,7-dihydrothieno[3,2-b]pyridine-6-carbonitrile

생성물 1

HCID 222566757-Chloro-2-phenylthieno[3,2-b]pyridine-6-carbonitrile

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

A mixture of 7-oxo-2-phenyl-4,7-dihydrothieno[3,2-b]pyridine-6-carbonitrile (878 mg, 3.48 mmol) and 10 mL of phosphorous oxychloride is heated at reflux for 1 hour. The reaction mixture is cooled to room temperature and hexane is added. The solids are collected by filtration and stirred with saturated aqueous sodium bicarbonate. The solids are collected by filtration washing with water, ethyl acetate and methanol to provide 751 mg of 7-chloro-2-phenylthieno[3,2-b]pyridine-6-carbonitrile that is not purified.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 1 hour
  3. filtrationThe solids are collected by filtration
  4. filtrationThe solids are collected by filtration
  5. washwashing with water, ethyl acetate and methanol

출처 및 근거

ORD 기록
ord-7097db4301734b9c865aa3e952ab17ad
출처 데이터셋
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06987116B2

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