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

HRID 1695234

反応式

HRID 1695234 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-009cc470c01b4f7bba83b356848fb8bf
出典データセット
uspto-grants-2012_04
特許番号
US08163729B2

関連ノート

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