Ammonia → HCID 21487720, compound

HRID 1076592Notes

Reaction equation

HRID 1076592 reaction equation
[CH3:1][N:2]1[C:7]2[S:8][CH:9]=[C:10]([CH3:11])[C:6]=2[C:5]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[N:4][C:3]1=[O:18].S(Cl)([Cl:22])(=O)=O.N>C(Cl)(Cl)Cl>[CH3:1][N:2]1[C:7]2[S:8][C:9]([Cl:22])=[C:10]([CH3:11])[C:6]=2[C:5]([C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[N:4][C:3]1=[O:18]

Participants

5

Reactant 3

HCID 222AmmoniaHCID 24648Sulfuryl chlorideHCID 21487718HCID 21487718, compound

Product 1

HCID 21487720HCID 21487720, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent2×

Procedure

To a solution of 1.33 g of 1-methyl-4-phenyl-5-methyl-1,2-dihyrothieno[2,3-d] -pyrimidin-2-one in 35 of chloroform is added dropwise 1.62 g of sulfuryl chloride in 6 ml of chloroform. After stirring the reaction mixture for 5 hours at room temperature, the reaction mixture is neutralized with aqueous ammonia and then extracted with chloroform. The chloroform extracts are washed with water, dried, evaporated under reduced pressure to a residue to give crystals of 1-methyl-4-phenyl-5-methyl-6-chloro-1,2-dihydrothieno[2,3-d]pyrimidin-2-one, which are recrystallized from ethanol-ether to give crystals having a melting point of 190° - 191.5°C.

Workup

  1. extractionextracted with chloroform
  2. washThe chloroform extracts are washed with water
  3. customdried
  4. customevaporated under reduced pressure to a residue

Sources & evidence

ORD record
ord-4663a3fc75a0412b9118877d268e69d0
Source dataset
uspto-grants-1976_05
Patent number
US03957783

Reaction notes

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