Hydrochloric Acid → HCID 66733850、化合物

HRID 1913229ノート

反応式

HRID 1913229 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.Cl>C(Cl)Cl.O1CCOCC1>[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

7

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 962WaterHCID 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 2

HCID 6344Dichloromethane溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

In a 40 mL scintillation vial was combined 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-amine (Int-5g, 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 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 were dried over Na2SO4 and the solvent was removed in vacuo to yield 4-(7-aminopyrazolo[1,5-a]pyrimidin-5-yl)cyclohexanone (Int-5h) (1.18 g, 93% yield) as a pale orange solid.

後処理

  1. customThe vial was capped
  2. customsealed
  3. temperaturethe reaction 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 were dried over Na2SO4
  7. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-920a11ede20f46499615c82af0b3ed8f
出典データセット
uspto-grants-2013_12
特許番号
US08609675B2

反応ノート

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