Hydrochloric Acid → HCID 21896882、化合物

HRID 719122ノート

反応式

HRID 719122 の反応式
[ClH:1].[CH2:2]([O:4][C:5]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:6]=1[C:7]#[N:8])[CH3:3].[CH2:15]([OH:17])[CH3:16]>>[ClH:1].[CH2:2]([O:4][C:5]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[CH:9][C:6]=1[C:7](=[NH:8])[O:17][CH2:15][CH3:16])[CH3:3]

参加物

4

反応物 3

HCID 313Hydrochloric Acid2 回HCID 702EthanolHCID 218969052-Ethoxy-4-methoxybenzonitrile

生成物 1

HCID 21896882HCID 21896882、化合物収率 79%

反応条件

温度
-10 °C

実験手順

Hydrogen chloride gas was passed through a solution of 2-ethoxy-4-methoxy-benzonitrile (6.3 g, 35.55 mmol) in anhydrous ethanol (70 mL) cooled to −10° C. After 30 min, hydrogen chloride gas was stopped and the reaction mixture was stirred at room temperature in a closed reaction vessel for 4 d. 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-ethoxy-4-methoxy-benzimidate hydrochloride (7.3 g, 79%). 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-1cbf5cb58a3f420389ba7b092e4888e9
出典データセット
uspto-grants-2006_11
特許番号
US07132421B2

反応ノート

読み込み中…