tert-butyl 2-cyano-2-(1-methyl-1H-pyrazol-5-yl)acetate → 2-(1-methyl-1H-pyrazol-5-yl)acetonitrile

HRID 931132ノート

反応式

HRID 931132 の反応式
[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

反応物 1

HCID 117966348tert-butyl 2-cyano-2-(1-methyl-1H-pyrazol-5-yl)acetate

生成物 1

HCID 252483742-(1-methyl-1H-pyrazol-5-yl)acetonitrile収率 95.9%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 135291,1,1,3,3,3-Hexafluoro-2-propanol溶媒

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

  1. customat 130° C.
  2. customfor 15 minutes
  3. washwashed with water (5 mL) and brine (5 mL)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. 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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