Formic Acid → HCID 178481857、化合物
反応式
[F:1][CH:2]([F:11])[C:3](=O)[CH2:4][C:5](OCC)=[O:6].C(O)=O.[CH3:15][NH:16][NH2:17]>C(OC)(C)(C)C>[CH3:15][N:16]1[C:5]([OH:6])=[CH:4][C:3]([CH:2]([F:11])[F:1])=[N:17]1参加物
5
反応条件
- 温度
- 5 °C
実験手順
166 g (1 mol) of ethyl difluoroacetoacetate are initially charged in 500 ml of methyl tert-butyl ether, and 140 g of formic acid are added. After the mixture has been cooled to 5° C., 119 g of methylhydrazine are added in 40% aqueous solution. The mixture is stirred at 22° C. for a further 20 h. The phases are separated, and the organic phase is washed with 200 ml of water and dried over MgSO4. After the solvent has been removed under reduced pressure, 148 g of the product are obtained as a yellow solid with an m.p. of 133° C. and a purity of 95%. Yield 95%.
後処理
- customThe phases are separated
- washthe organic phase is washed with 200 ml of water
- dry with materialdried over MgSO4
- customAfter the solvent has been removed under reduced pressure, 148 g of the product
- customare obtained as a yellow solid with an m.p. of 133° C.
出典と根拠
- ORDレコード
- ord-a5a259a8080d4d6aa13f5e2c7b005b8a
- 出典データセット
- uspto-grants-2013_06
- 特許番号
- US08455664B2
反応ノート
読み込み中…