Phosphorus sulfide (P2S5) → HCID 12521655, compound

HRID 371636Notes

Reaction equation

HRID 371636 reaction equation
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[NH:6][C:7](=O)[C:8]3[C:9](=[CH:11][S:12][CH:13]=3)[NH:10][C:4]=2[CH:3]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:18]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[NH:6][C:7](=[S:18])[C:8]3[C:9](=[CH:11][S:12][CH:13]=3)[NH:10][C:4]=2[CH:3]=1

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 12521645HCID 12521645, compound

Product 1

HCID 12521655HCID 12521655, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A mixture of 0.88 g. of 6-chloro-4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one and 1.0 g. of phosphorus pentasulfide in 10 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 20 ml. of 1N sodium carbonate solution (pH 7-7.2) for 18 hours. The precipitate is collected, washed with water and recrystallized from methanol to give an orange solid, m.p. 235°-237° C. (dec.).

Workup

  1. additionA mixture of 0.88 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 an orange solid, m.p. 235°-237° C. (dec.)

Sources & evidence

ORD record
ord-3ff248a6486f4e368b17e7aeda33d692
Source dataset
uspto-grants-1978_05
Patent number
US04087421

Reaction notes

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