二氯甲烷 → 2-Methylene-3-quinuclidone

HRID 347657

反应方程式

HRID 347657 反应方程式
Cl.O.O.[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2.C([O-])([O-])=O.[K+].[K+].C(Cl)Cl>O>[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2

参与物

5

反应物 3

HCID 6344二氯甲烷HCID 11430碳酸钾HCID 219542752-Methylene-3-quinuclidinone dihydrate hydrochloride

产物 1

HCID 3229732-Methylene-3-quinuclidone收率 100%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

A mixture of 2-methylene-3-quinuclidinone dihydrate hydrochloride (27.2 g, 0.13 mol, 1 eq) and K2CO3 (86.0 g, 0.62 mol, 4.8 eq) is dissolved in 130 mL water and 250 mL CH2Cl2 and stirred vigorously. After 3 days, the layers are separated and the aqueous layer is extracted with CH2Cl2. The combined organic layers are dried (MgSO4), filtered and concentrated to give 17.8 g (100%) of 2-methylenequinuclidin3-one as a yellow oil. MS (ESI) for C8H11NO m/z 138.1 (M+).

后处理

  1. customthe layers are separated
  2. extractionthe aqueous layer is extracted with CH2Cl2
  3. dry with materialThe combined organic layers are dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

来源与证据

ORD记录
ord-97963cac6149420c81d4ebb0fdaae399
来源数据集
uspto-grants-2007_02
专利号
US07176198B2

关联笔记

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