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

HRID 2107628ノート

反応式

HRID 2107628 の反応式
[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]

参加物

4

反応物 3

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

生成物 1

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

実験手順

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°.

後処理

  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°

出典と根拠

ORDレコード
ord-15da17b956644bc9abb72f70f4cce27c
出典データセット
uspto-grants-1990_06
特許番号
US04935431

反応ノート

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