Hydrochloric Acid → 1-tert-Butyl-1H-pyrazole

HRID 57845

反応式

HRID 57845 の反応式
CO[CH:3](OC)[CH2:4][CH:5](OC)OC.Cl.[C:13]([NH:17][NH2:18])([CH3:16])([CH3:15])[CH3:14].Cl.O>CCO>[C:13]([N:17]1[CH:5]=[CH:4][CH:3]=[N:18]1)([CH3:16])([CH3:15])[CH3:14]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 66019TetramethoxypropaneHCID 81889tert-Butylhydrazine monohydrochloride

生成物 1

HCID 134698151-tert-Butyl-1H-pyrazole収率 89.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1,1,3,3-tetramethoxypropane (3.7 g, 22.6 mmol), tert-butylhydrazine hydrochloride (2.8 g, 22.6 mmol), and conc. HCl (6 mL, 72 mmol) in EtOH (30 mL) was heated at reflux overnight. The reaction mixture was poured into water and the resulting mixture was extracted with ether (30 mL×3). The combined organics was washed with brine (20 mL), dried over MgSO4, and concentrated under reduced pressure to afford 1-tert-butyl-1H-pyrazole as a white solid (2.5 g, 89%). MS (ESI) m/z: 125 [M+H]+.

後処理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. extractionthe resulting mixture was extracted with ether (30 mL×3)
  4. washThe combined organics was washed with brine (20 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-6a335cf3c39a4015825d004aca41beae
出典データセット
uspto-grants-2016_09
特許番号
US09434725B2

関連ノート

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