Phosphorus sulfide (P2S5) → HCID 135848425, compound

HRID 262971Notes

Reaction equation

HRID 262971 reaction equation
[C:1]1([C:7]2[C:8]3[CH:17]=[CH:16][S:15][C:9]=3[NH:10][C:11](=O)[CH2:12][N:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:19]>N1C=CC=CC=1>[C:1]1([C:7]2[C:8]3[CH:17]=[CH:16][S:15][C:9]=3[NH:10][C:11](=[S:19])[CH2:12][N:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 13558422330199-04-3

Product 1

HCID 135848425HCID 135848425, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

12.1 g (0.05 mol) of 1,3-dihydro-5-phenyl-2H-thieno[2,3-e]-1,4-diazepin-2-one are heated to reflux for 35 minutes with 12.2 g (0.055 mol) of phosphorus pentasulphide in 400 ml of absolute pyridine, dry nitrogen being conducted through the solution. The solution is concentrated to 200 ml and the mixture separated on a 70 cm long column (φ3.5 cm) filled with 250 g of Silica gel [0.05 to 0.2 mm (Merck)]. The solution is concentrated under a vacuum and yields 1,3-dihydro-5-phenyl-2H-thieno[2,3-e]-1,4-diazepine-2-thione in the form of yellow crystals, melting point 208°-210° C.

Workup

  1. concentrationThe solution is concentrated to 200 ml
  2. customthe mixture separated on a 70 cm long column (φ3.5 cm)
  3. additionfilled with 250 g of Silica gel [0.05 to 0.2 mm (Merck)]
  4. concentrationThe solution is concentrated under a vacuum

Sources & evidence

ORD record
ord-841c8fd1d96c481290a89bf314add93c
Source dataset
uspto-grants-1979_05
Patent number
US04155913

Reaction notes

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