Pyridine → HCID 11446993、化合物
反応式
[S:1]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[C:5](=O)[NH:4][CH2:3][CH2:2]1.N1C=CC=CC=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:19]>O>[S:1]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[C:5](=[S:19])[NH:4][CH2:3][CH2:2]1参加物
5
実験手順
acb) 1.0 g of 3,4-dihydro-thieno[2,3-f][1,4]thiazepin-5(2H)-one was heated under reflux for 5 hours together with 15 ml of pyridine and 1.35 g of phosphorus pentasulfide. After cooling the mixture was poured into 90 ml of water and the crystals were removed by filtration. After chromatography on silica gel, the product was recrystallized from ethyl acetate. There was obtained 3,4-dihydro-thieno-[2,3-f][1,4]thiazepine-5(2H)-thione as yellow crystals of m.p. 138°-139°.
後処理
- temperatureAfter cooling the mixture
- customthe crystals were removed by filtration
- customAfter chromatography on silica gel, the product was recrystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-dc576e5ee68a4c968338699e8711b18c
- 出典データセット
- uspto-grants-1991_07
- 特許番号
- US05036066
反応ノート
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