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

HRID 2408335

반응식

HRID 2408335 반응식
[Cl:1][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.C(=O)([O-])[O-].[Cs+].[Cs+].CC1C=CC(S(O[CH2:31][CH2:32][O:33][CH:34]([CH3:36])[CH3:35])(=O)=O)=CC=1.O>CC#N.C(OCC)(=O)C>[Cl:1][C:2]1[N:3]=[C:4]2[N:11]([CH2:31][CH2:32][O:33][CH:34]([CH3:36])[CH3:35])[C:10]([CH3:13])([CH3:12])[CH2:9][N:5]2[C:6](=[O:8])[CH:7]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 19099443HCID 19099443, 화합물HCID 1363591007-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

생성물 1

HCID 680345397-chloro-1-(2-isopropoxyethyl)-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one수율 59.4%

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

반응 조건

온도
65 °C

실험 절차

To 0.200 g of 7-chloro-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one suspended in 7 mL of CH3CN, 0.65 g of cesium carbonate and 0.51 g of 2-isopropoxyethyl 4-methylbenzenesulfonate are added. The mixture is heated to 65° C. for 36 h. Water, ethyl acetate are added and then after decantation, the organic phase is dried with magnesium sulfate and then evaporated. The crude is purified by flash chromatography on silica gel (CH2Cl2/MeOH, 99/1). 0.17 g (yield=45%) of 7-chloro-1-(2-isopropoxyethyl)-2,2-dimethyl-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one are obtained as a brown powder.

후처리

  1. dry with materialafter decantation, the organic phase is dried with magnesium sulfate
  2. customevaporated
  3. customThe crude is purified by flash chromatography on silica gel (CH2Cl2/MeOH, 99/1)

출처 및 근거

ORD 기록
ord-ccf501ae24a54f1397e08b43a7be80bf
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08815853B2

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