反応式
[OH-].[OH:2][C:3]1[N+:7]2[CH2:8][CH2:9][C:10]3[CH:14]=[CH:13][S:12][C:11]=3[C:6]=2S[C:4]=1[C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([F:21])[CH:16]=1.[CH3:22][C:23](=[O:26])[C:24]#[CH:25]>C1(C)C=CC=CC=1>[C:23]([C:24]1[CH:25]=[C:4]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([F:21])[CH:16]=2)[C:3](=[O:2])[N:7]2[C:6]=1[C:11]1[S:12][CH:13]=[CH:14][C:10]=1[CH2:9][CH2:8]2)(=[O:26])[CH3:22]参加物
4
実験手順
A solution of 0.303 g of 5,6-dihydro-3-hydroxy-2-(m-fluorophenyl)-thiazolo-[3,2-a]thieno[2,3-c]pyridinium hydroxide (internal salt) and 0.145 ml of 3-butyn-2-one in 5 ml of toluene was heated under reflux for 1 hour. The solvent is evaporated in vacuo and the residue is chromatographed over silica gel with toluene/ethyl acetate (1:1). After recrystallization from ethanol, there was obtained 10-acetyl-4,5-dihydro-8-(m-fluorophenyl)-7H-thieno[2,3-a]quinolizin-7-one of m.p. 109°-110°.
後処理
- temperatureunder reflux for 1 hour
- customThe solvent is evaporated in vacuo
- customthe residue is chromatographed over silica gel with toluene/ethyl acetate (1:1)
- customAfter recrystallization from ethanol
出典と根拠
- ORDレコード
- ord-5c5089c2827e4d309a6486d40cd3740f
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04889848
関連ノート
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