Phosphorus sulfide (P2S5) → HCID 88786584, compound

HRID 1395013Notes

Reaction equation

HRID 1395013 reaction equation
[Br:1][C:2]1[S:18](=O)[C:5]2[O:6][CH:7]=[CH:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:21].C([O-])(O)=O.[Na+]>COCCOCCOC>[Br:1][C:2]1[S:18][C:5]2[O:6][C:7](=[S:21])[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[Cl:17])[C:4]=2[CH:3]=1

Participants

5

Reactant 3

HCID 14817Phosphorus sulfide (P2S5)HCID 516892Sodium BicarbonateHCID 70596624HCID 70596624, compound

Product 1

HCID 88786584HCID 88786584, compound

Reagents, catalysts & solvents 1

HCID 8150DiglymeSolvent

Procedure

(a) 0.1 Mol=35.8 gm of 7-bromo-5-(o-chlorophenyl)-thieno-[2,3-e]-4,1-oxazepinone were heated with 350 ml of diglyme, 24 gm of P2S5 and 19 gm of NaHCO3 for 30 minutes at 60° C. Subsequently, the reaction mixture was poured over about 1 liter of ice water, whereby a crystalline precipitate was formed, which was suction-filtered off, washed with water and dried. 37 gm=99% of theory of 7-bromo-5-(o-chlorophenyl)-thieno-[2,3-e]-4,1-oxazepine-2-thione were obtained M.p. from 200° C. (decomp.).

Workup

  1. customwas formed
  2. filtrationwhich was suction-filtered off
  3. washwashed with water
  4. customdried

Sources & evidence

ORD record
ord-dd78d1e6cde7438bb6e036fe3c95ee12
Source dataset
uspto-grants-1980_05
Patent number
US04201712

Reaction notes

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