Phosphorus sulfide (P2S5) → HCID 12521656, compound

HRID 371640Notes

Reaction equation

HRID 371640 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH3:12])[C:10]3=[CH:13][S:14][CH:15]=[C:9]3[C:8](=O)[NH:7][C:6]=2[CH:17]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:19]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH3:12])[C:10]3=[CH:13][S:14][CH:15]=[C:9]3[C:8](=[S:19])[NH:7][C:6]=2[CH:17]=1

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 12521646HCID 12521646, compound

Product 1

HCID 12521656HCID 12521656, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A mixture of 0.5 g. of 7-chloro-4-methyl-4,9-dihydro-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 mixture is concentrated to dryness and 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 a yellow solid, m.p. 238°-240° C.

Workup

  1. additionA mixture of 0.5 g
  2. temperatureheated
  3. temperatureunder reflux for 4 hours
  4. concentrationThe mixture is concentrated to dryness
  5. customThe precipitate is collected
  6. washwashed with water
  7. customrecrystallized from methanol
  8. customto give a yellow solid, m.p. 238°-240° C.

Sources & evidence

ORD record
ord-074211da42f142ce9db36146a1fb0abc
Source dataset
uspto-grants-1978_05
Patent number
US04087421

Reaction notes

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