Dimethylformamide dimethyl acetal → HCID 178484244、化合物

HRID 452972

反応式

HRID 452972 の反応式
[C:1]([C:5]1[CH:9]=[C:8]([NH2:10])[NH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].CO[CH:13](OC)[N:14]([CH3:16])[CH3:15]>>[C:1]([C:5]1[CH:9]=[C:8](/[N:10]=[CH:13]/[N:14]([CH3:16])[CH3:15])[NH:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

3

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 178441179HCID 178441179、化合物

生成物 1

HCID 178484244HCID 178484244、化合物収率 99%

実験手順

A mixture of 3-tert-butyl-1H-pyrazol-5-amine (5 g, 36 mmol, Alfa-aesar) and N,N-dimethylformamide dimethylacetal (153 mL, 1078 mmol, Aldrich) was refluxed overnight. The reaction mixture was then cooled, concentrated under reduced pressure and the residue was purified by column chromatography using an Analogix® Intelliflash280™ (SiO2, 0-5% methanol in dichloromethane) to provide 6.9 g (99%) of the title compound. MS (ESI+) m/z 195 (M+H)+.

後処理

  1. temperaturewas refluxed overnight
  2. temperatureThe reaction mixture was then cooled
  3. concentrationconcentrated under reduced pressure
  4. customthe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-ab140c35fa8047ea8097a7d65dc39f06
出典データセット
uspto-grants-2013_07
特許番号
US08492371B2

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