Dichloromethane → 2-Methylene-3-quinuclidone

HRID 347657

反応式

HRID 347657 の反応式
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

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 219542752-Methylene-3-quinuclidinone dihydrate hydrochloride

生成物 1

HCID 3229732-Methylene-3-quinuclidone収率 100%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-97963cac6149420c81d4ebb0fdaae399
出典データセット
uspto-grants-2007_02
特許番号
US07176198B2

関連ノート

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