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

HRID 57845

반응식

HRID 57845 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 134698151-tert-Butyl-1H-pyrazole수율 89.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-6a335cf3c39a4015825d004aca41beae
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434725B2

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