Carbonic acid sodium salt (1:2) → N-环丙基甲基-4-哌啶酮

HRID 272557

反应方程式

HRID 272557 反应方程式
Br[CH2:2][CH:3]1[CH2:5][CH2:4]1.Cl.O.[NH:8]1[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][CH2:9]1.C(=O)([O-])[O-].[Na+].[Na+]>C(#N)C>[CH:5]1([CH2:4][N:8]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][CH2:9]2)[CH2:3][CH2:2]1

参与物

5

反应物 3

HCID 10340Carbonic acid sodium salt (1:2)HCID 81503溴甲基环丙烷HCID 27239014-哌啶酮一水合物盐酸盐

产物 1

HCID 18002181N-环丙基甲基-4-哌啶酮收率 55.3%

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

反应条件

温度
85 °C

实验过程

To a suspension of bromomethyl cyclopropane (4 mmol) and 4-piperidone hydrate hydrochloride (4 mmol) in acetonitrile (30 mL) was added sodium carbonate (11 mmol). The reaction mixture was stirred 16 h at 85° C. The resulting suspension was filtered and the solid was washed with acetonitrile. The filtrate was concentrated in vacuo and purified by column chromatography on silica eluting with DCM/2N NH3 in methanol 97:3 to yield 339 mg of the title compound as yellow oil. MS (m/e): 154.2 (MH+, 100%).

后处理

  1. filtrationThe resulting suspension was filtered
  2. washthe solid was washed with acetonitrile
  3. concentrationThe filtrate was concentrated in vacuo
  4. custompurified by column chromatography on silica eluting with DCM/2N NH3 in methanol 97:3

来源与证据

ORD记录
ord-6f8c09e36221499a9402e63f834e28db
来源数据集
uspto-grants-2008_11
专利号
US07456174B2

关联笔记

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