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

HRID 2408335

反応式

HRID 2408335 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
65 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-ccf501ae24a54f1397e08b43a7be80bf
出典データセット
uspto-grants-2014_08
特許番号
US08815853B2

関連ノート

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