Pyridine → HCID 11446993, 화합물
반응식
[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]1참가 물질
5
실험 절차
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°.
후처리
- temperatureAfter cooling the mixture
- customthe crystals were removed by filtration
- customAfter chromatography on silica gel, the product was recrystallized from ethyl acetate
출처 및 근거
- ORD 기록
- ord-dc576e5ee68a4c968338699e8711b18c
- 출처 데이터셋
- uspto-grants-1991_07
- 특허 번호
- US05036066
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