Phosphorus trichloride → HCID 15027704, compound

HRID 1090656Notes

Reaction equation

HRID 1090656 reaction equation
P(Cl)(Cl)Cl.[CH2:5]([N:12]1[C:22](=[O:23])[C:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[C:15]2[S:16](=O)[CH2:17][CH:18]=[CH:19][N:14]2[C:13]1=[O:30])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>CN(C=O)C>[CH2:5]([N:12]1[C:22](=[O:23])[C:21]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[C:15]2[S:16][CH2:17][CH:18]=[CH:19][N:14]2[C:13]1=[O:30])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

Participants

4

Reactant 2

HCID 24387Phosphorus trichlorideHCID 15027700HCID 15027700, compound

Product 1

HCID 15027704HCID 15027704, compoundYield 81.1%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
-10 °C

Procedure

Phosphorus trichloride (0.2 ml) was added dropwise to a solution of 7-benzyl-1-oxo-9-phenyl-2H,6H-pyrimido[6,1-b]-[1,3]thiazine-6,8(7H)-dione (0.4 g) in DMF (8 ml) under stirring at -10° C. The mixture was stirred at the same temperature for 30 minutes and the resulting solution was poured to ice-water to give crystals and the crystals were collected by filtration. The resulting crude crystals were washed and recrystalized from methylene chloride-methanol to give colorless needles (0.31 g, 81%).

Workup

  1. stirringThe mixture was stirred at the same temperature for 30 minutes
  2. customto give crystals
  3. filtrationthe crystals were collected by filtration
  4. washThe resulting crude crystals were washed
  5. customrecrystalized from methylene chloride-methanol

Sources & evidence

ORD record
ord-f381a497032f4ad7b4bd53048a1f7965
Source dataset
uspto-grants-1992_01
Patent number
US05082838

Reaction notes

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