Phosphorus sulfide (P2S5) → HCID 12521653, compound

HRID 1605907Notes

Reaction equation

HRID 1605907 reaction equation
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5](=O)[C:4]2=[CH:14][S:15][CH:16]=[C:3]12.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:18]>N1C=CC=CC=1>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5](=[S:18])[C:4]2=[CH:14][S:15][CH:16]=[C:3]12

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 125216424,9-Dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

Product 1

HCID 12521653HCID 12521653, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A mixture of 0.4 g. of 4,9-dihydro-4-methyl-10H-thieno[3,4-b] [1,5] benzodiazepin-10-one and 0.5 g. of phosphorus pentasulfide in 5 ml. of dry pyridine is stirred and heated under reflux for 4 hours. The reaction mixture is concentrated to dryness and the residue is stirred with 10 ml. of 1N sodium carbonate solution for 18 hours. The precipitate is collected, washed with water and recrystallized from methanol to give gold crystals, m.p. 203°-204°C.

Workup

  1. additionA mixture of 0.4 g
  2. temperatureheated
  3. temperatureunder reflux for 4 hours
  4. concentrationThe reaction mixture is concentrated to dryness
  5. customThe precipitate is collected
  6. washwashed with water
  7. customrecrystallized from methanol
  8. customto give gold crystals, m.p. 203°-204°C.

Sources & evidence

ORD record
ord-318453e843904468aae9be92cba5634e
Source dataset
uspto-grants-1976_04
Patent number
US03951981

Reaction notes

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