Ethanol → HCID 66733850、化合物

HRID 2047057ノート

反応式

HRID 2047057 の反応式
O1[C:5]2([CH2:10][CH2:9][CH:8]([C:11]3[CH:16]=[C:15]([NH2:17])[N:14]4[N:18]=[CH:19][CH:20]=[C:13]4[N:12]=3)[CH2:7][CH2:6]2)[O:4]CC1.CCO.O.O1CCOCC1>C(Cl)Cl>[NH2:17][C:15]1[N:14]2[N:18]=[CH:19][CH:20]=[C:13]2[N:12]=[C:11]([CH:8]2[CH2:7][CH2:6][C:5](=[O:4])[CH2:10][CH2:9]2)[CH:16]=1

参加物

6

反応物 4

HCID 702EthanolHCID 962WaterHCID 312751,4-DioxaneHCID 667334895-(1,4-Dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-amine

生成物 1

HCID 66733850HCID 66733850、化合物収率 93%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
80 °C

実験手順

In a 40 mL scintillation vial is combined 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-amine (5.54 mmol, 1.52 g), EtOH (10 mL), H2O (4 mL) and 4N HCL:dioxane (4 mL). The vial was capped, sealed and the reaction was heated to 80° C. overnight. After 18 hours, the reaction mixture was cooled to room temperature and diluted with DCM (100 mL). The solution was washed with saturated NaHCO3(aq) and extracted with DCM twice more. The combined organics are dried over Na2SO4 and the solvent removed in vacuo to yield 4-(7-aminopyrazolo[1,5-a]pyrimidin-5-yl)cyclohexanone (1.18 g, 93% yield) as pale orange solid.

後処理

  1. customThe vial was capped
  2. customsealed
  3. temperaturethe reaction mixture was cooled to room temperature
  4. washThe solution was washed with saturated NaHCO3(aq)
  5. extractionextracted with DCM twice more
  6. dry with materialThe combined organics are dried over Na2SO4
  7. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-2f55afef3ace4c72b94aa03ca1522551
出典データセット
uspto-grants-2013_11
特許番号
US08591943B2

反応ノート

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