Pyridine → HCID 11446993, compound
Reaction equation
[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]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
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°.
Workup
- temperatureAfter cooling the mixture
- customthe crystals were removed by filtration
- customAfter chromatography on silica gel, the product was recrystallized from ethyl acetate
Sources & evidence
- ORD record
- ord-a00e981f88424c42b98611bab4f9fcfb
- Source dataset
- uspto-grants-1994_06
- Patent number
- US05321021
Reaction notes
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