Phosphorus oxychloride → 7-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

HRID 2408336

반응식

HRID 2408336 반응식
O[C:2]1[N:3]=[C:4]2[NH:11][C:10]([CH3:13])([CH3:12])[CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1.O=P(Cl)(Cl)[Cl:16]>ClC(Cl)C>[Cl:16][C:2]1[N:3]=[C:4]2[NH:11][C:10]([CH3:13])([CH3:12])[CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 136269314HCID 136269314, 화합물

생성물 1

HCID 1363591007-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one수율 83%

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
60 °C

실험 절차

18.5 g of 7-hydroxy-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one are suspended in 200 mL of dichloroethane. 48 mL of POCl3 are added and the mixture is heated to 60° C. for 3 h. After returning to RT, the solvents are dry evaporated. The residue is taken up in water and AcOET, 30% NaOH is added until pH=12. The product precipitates, it is filtered and then dried. 16.9 g (yield=83%) of 7-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one are obtained as a yellow solid and including the following characteristics:

후처리

  1. customAfter returning to RT
  2. customthe solvents are dry
  3. customevaporated
  4. additionAcOET, 30% NaOH is added until pH=12
  5. customThe product precipitates
  6. filtrationit is filtered
  7. customdried

출처 및 근거

ORD 기록
ord-cfbad2d59f32478b9814e43839378362
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08815853B2

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