Phosphorus sulfide (P2S5) → HCID 20494272, compound
Reaction equation
[Cl:1][C:2]1[C:3](=O)[NH:4][C:5](=[O:9])[NH:6][C:7]=1[CH3:8].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:12]>O1CCOCC1>[Cl:1][C:2]1[C:3](=[S:12])[NH:4][C:5](=[O:9])[NH:6][C:7]=1[CH3:8]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
5-Chloro-6-methyluracil (prepared as described in Johnson, B. T. J. Amer. Chem. Soc. 65 (1943) (1220) (0.018 mol) and phosphorus pentasulphide (0.019 mol) were heated together in refluxing dioxan (200 ml) for 45 min. The hot reaction mixture was then filtered and the cold filtrate concentrated and diluted with ether. The participate collected after a few hours in the cold, was recrystallised from water; yield 75% m.p. 297°-300° C. (decomp.); (Found: C, 32.69; H, 3.96. Calc. for C5H5ClN2OS.1/2H2O: C, 32.35; H, 3.25).
Workup
- filtrationThe hot reaction mixture was then filtered
- concentrationthe cold filtrate concentrated
- additiondiluted with ether
- customThe participate collected after a few hours in the cold,
- customwas recrystallised from water
Sources & evidence
- ORD record
- ord-4144011a89304f38a047939c568a2deb
- Source dataset
- uspto-grants-1983_07
- Patent number
- US04395406
Reaction notes
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