Water → HCID 20213358, compound

HRID 1905869Notes

Reaction equation

HRID 1905869 reaction equation
[CH3:1][N:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([S:16][CH3:17])[CH:9]=2)=[CH:6][C:5](=O)[N:4]([CH3:19])[C:3]1=[O:20].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22].O>N1C=CC=CC=1>[CH3:1][N:2]1[C:7]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([S:16][CH3:17])[CH:9]=2)=[CH:6][C:5](=[S:22])[N:4]([CH3:19])[C:3]1=[O:20]

Participants

5

Reactant 3

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 20213354HCID 20213354, compound

Product 1

HCID 20213358HCID 20213358, compoundYield 159.3%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

To a suspension of 1,3-dimethyl-6-(4-methoxy-3-methylthiophenyl)-1,2,3,4-tetrahydropyrimidine-2,4dione (6.5 g) in pyridine (60 ml) was added phosphorus pentasulfide (4.95 g), and refluxed for 8 hours. After cooled, the mixture was poured into water (600 ml). The precipitates were collected, dried in the air, and refluxed with ethanol (150 ml) for 2 hours. After cooled, resulting precipitates were filtered, and washed with ethanol and diisopropyl ether, to give 1,3-dimethyl-6-(4-methoxy-3-methylthiophenyl)-1,2,3,4-tetrahydro-4-thioxopyrimidin-2-one (5.47 g). mp 174°-176° C.

Workup

  1. temperaturerefluxed for 8 hours
  2. temperatureAfter cooled
  3. customThe precipitates were collected
  4. customdried in the air
  5. temperaturerefluxed with ethanol (150 ml) for 2 hours
  6. temperatureAfter cooled
  7. customresulting
  8. customprecipitates
  9. filtrationwere filtered
  10. washwashed with ethanol and diisopropyl ether

Sources & evidence

ORD record
ord-2d93af03f1ec4d0bb3b85e7d67ff3b0d
Source dataset
uspto-grants-1987_03
Patent number
US04649142

Reaction notes

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