Pyridine → HCID 11446993, compound

HRID 1109582Notes

Reaction equation

HRID 1109582 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-a00e981f88424c42b98611bab4f9fcfb
Source dataset
uspto-grants-1994_06
Patent number
US05321021

Reaction notes

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