Lawesson's reagent → HCID 20515325, compound

HRID 67519Notes

Reaction equation

HRID 67519 reaction equation
[CH3:1][N:2]1[C:8](=O)[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:4]2[CH2:3]1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:31]2)=CC=1>C1(C)C=CC=CC=1>[CH3:1][N:2]1[C:8](=[S:31])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:4]2[CH2:3]1

Participants

4

Reactant 2

HCID 87949Lawesson's reagentHCID 127597Ro 14-7437

Product 1

HCID 20515325HCID 20515325, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

670 mg (2.3 mmol) of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate and 497 mg (1.23 mmol) of 2,4-bis(p-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulphide are heated to boiling under reflux for 2.5 hours in 5 ml of absolute toluene. The mixture is chromatographed on silica gel with ethyl acetate and there is obtained ethyl 5,6-dihydro-5-methyl-6-thioxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 164°-165° C.

Workup

  1. customThe mixture is chromatographed on silica gel with ethyl acetate

Sources & evidence

ORD record
ord-96b2ebf0aec74d66baa8144b700fc1c9
Source dataset
uspto-grants-1982_08
Patent number
US04346033

Reaction notes

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