Sodium Hydroxide → 6-Butyryl-7-chloro-3-methoxythieno[3,2-b]pyridine

HRID 2107628노트

반응식

HRID 2107628 반응식
[CH3:1][O:2][C:3]1[C:7]2[NH:8][CH:9]=[C:10]([C:13](=[O:17])[CH2:14][CH2:15][CH3:16])[C:11](=O)[C:6]=2[S:5][CH:4]=1.[OH-].[Na+].P(Cl)(Cl)([Cl:22])=O>>[C:13]([C:10]1[C:11]([Cl:22])=[C:6]2[S:5][CH:4]=[C:3]([O:2][CH3:1])[C:7]2=[N:8][CH:9]=1)(=[O:17])[CH2:14][CH2:15][CH3:16]

참가 물질

4

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 230461623-Methoxy-6-butyrylthieno[3,2-b]pyridin-7(4H)-one

생성물 1

HCID 230461496-Butyryl-7-chloro-3-methoxythieno[3,2-b]pyridine

실험 절차

3-Methoxy-6-butyrylthieno[3,2-b]pyridin-7(4H)-one (3 g) and phosphorus oxychloride (10 ml) were heated under reflux for one hour. The reaction mixture was poured onto ice water (100 g) stirred for 30 minutes and then basified with 40% sodium hydroxide solution cooling with ice, then extracted with chloroform (3×100 ml). The chloroform extracts were combined dried over magnesium sulphate, filtered and evaporated under reduced pressure to give a brown solid, 3.1 g, m.p. 76°-78°.

후처리

  1. temperatureunder reflux for one hour
  2. additionThe reaction mixture was poured onto ice water (100 g)
  3. temperaturecooling with ice
  4. extractionextracted with chloroform (3×100 ml)
  5. dry with materialThe chloroform extracts were combined dried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customto give a brown solid, 3.1 g, m.p. 76°-78°

출처 및 근거

ORD 기록
ord-15da17b956644bc9abb72f70f4cce27c
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04935431

반응 노트

불러오는 중…