Hydrochloric Acid → 4-(1-Methylethoxy)-beta-oxobenzenepropanenitrile

HRID 1695234

반응식

HRID 1695234 반응식
CO[C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH:11]([CH3:13])[CH3:12])=[CH:6][CH:5]=1.[H-].[Na+].[CH3:17][C:18]#[N:19].Cl>C1(C)C=CC=CC=1>[CH:11]([O:10][C:7]1[CH:6]=[CH:5][C:4]([C:3](=[O:14])[CH2:17][C:18]#[N:19])=[CH:9][CH:8]=1)([CH3:12])[CH3:13]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6342AcetonitrileHCID 24758Sodium hydrideHCID 3015807Methyl 4-(1-methylethoxy)benzoate

생성물 1

HCID 203875144-(1-Methylethoxy)-beta-oxobenzenepropanenitrile

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

To a solution of 4-Isopropoxy-benzoic acid methyl ester (2.2 g, 11.2 mmol, 1.0 eq) in dry toluene (15 mL) under N2, NaH (50-60% dispersion in mineral oil, 1.1 g, 22.4 mmol, 2.0 eq) was added. The mixture was heated at 80° C. and then dry CH3CN was added dropwise (2.8 mL, 56.0 mmol, 5.0 eq). The reaction was heated for 18 hours, then was allowed to cool down to room temperature and acidified with HCl 2N. The organic phase was recovered and 2.0 g of crude were obtained and it was used for cyclization without further purification.

후처리

  1. temperatureThe reaction was heated for 18 hours
  2. temperatureto cool down to room temperature
  3. customThe organic phase was recovered
  4. custom2.0 g of crude were obtained
  5. customit was used for cyclization without further purification

출처 및 근거

ORD 기록
ord-009cc470c01b4f7bba83b356848fb8bf
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163729B2

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