Pyridine → HCID 70352522, compound

HRID 477935Notes

Reaction equation

HRID 477935 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>O>[S:1]1[C:7]2[CH:8]=[CH:9][S:10][C:6]=2[CH2:5][NH:4][CH2:3][CH2:2]1

Participants

5

Reactant 3

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

Product 1

HCID 70352522HCID 70352522, 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-a81221e2625843d68877f59f630cb51c
Source dataset
uspto-grants-1989_12
Patent number
US04889848

Reaction notes

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