Phosphorus sulfide (P2S5) → HCID 21256521, compound

HRID 635794Notes

Reaction equation

HRID 635794 reaction equation
[CH2:1]([CH:3]1[C:8](=O)[NH:7][C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[O:4]1)[CH3:2].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:15]>N1C=CC=CC=1>[CH2:1]([CH:3]1[C:8](=[S:15])[NH:7][C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[O:4]1)[CH3:2]

Participants

4

Reactant 2

HCID 14817Phosphorus sulfide (P2S5)HCID 31555992-Ethyl-2H-benzo[b][1,4]oxazin-3(4H)-one

Product 1

HCID 21256521HCID 21256521, compoundYield 532.7%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

0.25 g of 2-ethyl-1,4-benzoxazin-3-one is stirred in 2 ml of pyridine with 95 mg of phosphorus pentasulfide. The reaction is completed by reflux-boiling. It is poured onto water, extracted with ethyl acetate, and the organic phase is washed with brine. It is dried with magnesium sulfate and concentrated by evaporation. After column chromatography with hexane/ethyl acetate, 220 mg of product results.

Workup

  1. temperatureby reflux-boiling
  2. additionIt is poured onto water
  3. extractionextracted with ethyl acetate
  4. washthe organic phase is washed with brine
  5. dry with materialIt is dried with magnesium sulfate
  6. concentrationconcentrated by evaporation

Sources & evidence

ORD record
ord-97f59d314a304465accf2e88423a266d
Source dataset
uspto-grants-2001_02
Patent number
US06191127B1

Reaction notes

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