tert-butyl 2-cyano-2-(1-methyl-1H-pyrazol-5-yl)acetate → 2-(1-methyl-1H-pyrazol-5-yl)acetonitrile
반응식
[C:1]([CH:3]([C:11]1[N:15]([CH3:16])[N:14]=[CH:13][CH:12]=1)C(OC(C)(C)C)=O)#[N:2]>FC(F)(F)C(O)C(F)(F)F.C(OCC)C>[CH3:16][N:15]1[C:11]([CH2:3][C:1]#[N:2])=[CH:12][CH:13]=[N:14]1참가 물질
4
실험 절차
A mixture of tert-butyl 2-cyano-2-(1-methyl-1H-pyrazol-5-yl)acetate (130 mg, 0.588 mmol) in hexafluoroisopropanol (1 mL) was submitted to microwave radiation at 130° C. for 15 minutes. The reaction mixture was diluted with diethyl ether (30 mL), washed with water (5 mL) and brine (5 mL), dried over magnesium sulfate, filtered, concentrated under reduced pressure and dried under high vacuum to afford 2-(1-methyl-1H-pyrazol-5-yl)acetonitrile (68.3 mg) as a pale yellow oil. 1H NMR (500 MHz, CDCl3) δ 3.77 (s, 2H), 3.89 (s, 3H), 6.30 (s, 1H), 7.45 (s, 1H).
후처리
- customat 130° C.
- customfor 15 minutes
- washwashed with water (5 mL) and brine (5 mL)
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customdried under high vacuum
출처 및 근거
- ORD 기록
- ord-8fca63e6286b461b813c8aaf08cf8713
- 출처 데이터셋
- uspto-grants-2016_03
- 특허 번호
- US09296745B2
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