Acetic Acid → HCID 178481857, 화합물
반응식
[F:1][CH:2]([F:11])[C:3](=O)[CH2:4][C:5](OCC)=[O:6].C(O)(=O)C.[CH3:16][NH:17][NH2:18]>C(OC)(C)(C)C>[CH3:16][N:17]1[C:5]([OH:6])=[CH:4][C:3]([CH:2]([F:11])[F:1])=[N:18]1참가 물질
5
반응 조건
- 온도
- 5 °C
실험 절차
166 g (1 mol) of ethyl difluoroacetoacetate are initially charged in 500 ml of methyl tert-butyl ether, and 60 g of acetic 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, 140 g of the product are obtained as a yellow solid with an m.p. of 133° C. and a purity of 96%. Yield 91%.
후처리
- 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, 140 g of the product
- customare obtained as a yellow solid with an m.p. of 133° C.
출처 및 근거
- ORD 기록
- ord-850387ac8d2d4c15a70af626a39fd842
- 출처 데이터셋
- uspto-grants-2013_06
- 특허 번호
- US08455664B2
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