tert-butyl 2-cyano-2-(1-methyl-1H-pyrazol-5-yl)acetate → 2-(1-methyl-1H-pyrazol-5-yl)acetonitrile
反応式
[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]1参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-8fca63e6286b461b813c8aaf08cf8713
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09296745B2
反応ノート
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