Hydrochloric Acid → Ethyl 2-isopropoxy-4-methoxybenzimidate hydrochloride

HRID 1167304ノート

反応式

HRID 1167304 の反応式
[ClH:1].[CH:2]([O:5][C:6]1[CH:13]=[C:12]([O:14][CH3:15])[CH:11]=[CH:10][C:7]=1[C:8]#[N:9])([CH3:4])[CH3:3].[CH2:16]([OH:18])[CH3:17]>>[ClH:1].[CH:2]([O:5][C:6]1[CH:13]=[C:12]([O:14][CH3:15])[CH:11]=[CH:10][C:7]=1[C:8](=[NH:9])[O:18][CH2:16][CH3:17])([CH3:4])[CH3:3]

参加物

4

反応物 3

HCID 313Hydrochloric Acid2 回HCID 702EthanolHCID 227210812-Isopropoxy-4-methoxybenzonitrile

生成物 1

HCID 21896893Ethyl 2-isopropoxy-4-methoxybenzimidate hydrochloride収率 99%

反応条件

温度
-10 °C

実験手順

Hydrogen chloride gas was passed through a solution of 2-isopropoxy-4-methoxy-benzonitrile (11.5 g, 60.14 mmol) in anhydrous ethanol (250 mL) cooled to −10° C. After 45 min, hydrogen chloride gas was stopped and the reaction mixture was stirred at room temperature in a closed reaction vessel for 2 weeks. The reaction vessel was cooled to 0° C. before the stopper was removed. Argon gas was passed through the solution to remove excess hydrogen chloride gas. The solvent was evaporated and the residue was triturated in diethyl ether (100 mL) to afford ethyl 2-isopropoxy-4-methoxy-benzimidate hydrochloride (16.3 g, 99%). It was used without further purification.

後処理

  1. temperatureThe reaction vessel was cooled to 0° C. before the stopper
  2. customwas removed
  3. customto remove excess hydrogen chloride gas
  4. customThe solvent was evaporated
  5. customthe residue was triturated in diethyl ether (100 mL)

出典と根拠

ORDレコード
ord-569752e827a34fd0a523bb50db91fa0e
出典データセット
uspto-grants-2003_09
特許番号
US06617346B1

反応ノート

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