Ethyl diazoacetate → Ethyl (dicyclopropylmethoxy)acetate
反応式
[CH:1]1([CH:4]([CH:6]2[CH2:8][CH2:7]2)[OH:5])[CH2:3][CH2:2]1.[N+](=[CH:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[N-]>ClCCl.CCCCCCC.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.[Rh].[Rh]>[CH2:15]([O:14][C:12](=[O:13])[CH2:11][O:5][CH:4]([CH:6]1[CH2:8][CH2:7]1)[CH:1]1[CH2:3][CH2:2]1)[CH3:16]参加物
6
実験手順
To a solution of dicyclopropylmethan-1-ol (1.5 mL, 12.7 mmol) in dichloromethane (20 mL) is added rhodium (II) acetate dimer (10 mg) followed by ethyl diazoacetate (1.26 mL, 12.0 mmol). The reaction mixture is stirred at rt for 48 h. The reaction mixture is diluted with heptane, and filtered. The filtrate is evaporated, and the residue is vacuum distilled at 170° C. to give 1.24 g of the product 448.
後処理
- filtrationfiltered
- customThe filtrate is evaporated
- distillationdistilled at 170° C.
出典と根拠
- ORDレコード
- ord-3b96a48cc5554c38937449e8fff31ec8
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07741493B2
反応ノート
読み込み中…