Pyridine → HCID 11446993, compound

HRID 1087550Notes

Reaction equation

HRID 1087550 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]1

Participants

5

Reactant 3

HCID 1049PyridineHCID 14817Phosphorus sulfide (P2S5)HCID 11469493HCID 11469493, compound

Product 1

HCID 11446993HCID 11446993, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

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

  1. temperatureAfter cooling the mixture
  2. customthe crystals were removed by filtration
  3. customAfter chromatography on silica gel, the product was recrystallized from ethyl acetate

Sources & evidence

ORD record
ord-dc576e5ee68a4c968338699e8711b18c
Source dataset
uspto-grants-1991_07
Patent number
US05036066

Reaction notes

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