反応式
[CH2:1]([O:3][C:4]([C:6]1([CH2:9][OH:10])[CH2:8][CH2:7]1)=[O:5])[CH3:2].C(=O)([O-])O.[Na+].CC1(C)N([O])C(C)(C)CCC1.[Br-].[Na+].Cl[O-].[Na+].S([O-])([O-])(=O)=S.[Na+].[Na+]>ClCCl>[CH:9]([C:6]1([C:4]([O:3][CH2:1][CH3:2])=[O:5])[CH2:8][CH2:7]1)=[O:10]参加物
8
実験手順
To a solution of Preparation 232 1-hydroxymethyl-cyclopropanecarboxylic acid ethyl ester (3.00 g, 21.00 mmol) in dichloromethane (50 ml), at 0° C., was added saturated sodium hydrogen carbonate solution (50 ml), followed by TEMPO (659 mg, 4.00 mmol) and sodium bromide (400 mg, 4.00 mmol). After stirring for 5 min, sodium hypochlorite solution (10%, 14.00 mmol) was added slowly, followed by saturated sodium thiosulphate solution (50 ml). The two layers were separated and the aqueous layer was extracted with dichloromethane. The combined organic phases were dried (MgSO4) and concentrated in vacuo to give the titled compound (3.00 g).
後処理
- customThe two layers were separated
- extractionthe aqueous layer was extracted with dichloromethane
- dry with materialThe combined organic phases were dried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-46dfd3ebaae1485283626fa6d6d3ca1d
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07538134B2
関連ノート
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