Phosphorus sulfide (P2S5) → HCID 12521653, compound

HRID 371631Notes

Reaction equation

HRID 371631 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-ac9efb257ab74e67a76d313be6b0f3e1
Source dataset
uspto-grants-1978_05
Patent number
US04087421

Reaction notes

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