Phosphorus sulfide (P2S5) → HCID 14626777, compound

HRID 330471Notes

Reaction equation

HRID 330471 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=O)[CH2:9][N:8]3[C:13]4[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=4[CH:19]=[C:7]3[C:6]=2[CH:20]=1.C(=O)(O)[O-].[Na+].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:27]>COCCOCCOC.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[S:27])[CH2:9][N:8]3[C:13]4[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=4[CH:19]=[C:7]3[C:6]=2[CH:20]=1

Participants

6

Reactant 3

HCID 14817Phosphorus sulfide (P2S5)HCID 516892Sodium BicarbonateHCID 14854877HCID 14854877, compound

Product 1

HCID 14626777HCID 14626777, compoundYield 40%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8150DiglymeSolvent

Procedure

A mixture of 3.74 g 2-chloroindolo[1,2-d][1,4]benzodiazepin-6(7H)-one, 2.58 g sodium bicarbonate, and 13.67 g P2S5 in 85 ml diglyme was heated at 105°-120° C. under nitrogen for one and a half hours. The cooled reaction mixture was diluted with water to precipiate a solid. Recrystallization from toluene yielded 1.58 g solid, which decomposed at 265° C.

Workup

  1. temperaturewas heated at 105°-120° C. under nitrogen for one and a half hours
  2. customThe cooled reaction mixture
  3. customRecrystallization from toluene

Sources & evidence

ORD record
ord-9cd09e9ffbf546fe87063b5b0e7ca649
Source dataset
uspto-grants-1990_01
Patent number
US04897392

Reaction notes

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