Hydrochloric Acid → Benzamide

HRID 236869ノート

反応式

HRID 236869 の反応式
Cl[C:2]1[CH:3]=[CH:4][C:5](OC)=[C:6]([CH:10]=1)[C:7](Cl)=[O:8].Cl.C(C1C=CC(CC[NH2:24])=CC=1)C.N1C=CC=CC=1.Cl>C1(C)C=CC=CC=1.O>[C:7]([NH2:24])(=[O:8])[C:6]1[CH:5]=[CH:4][CH:3]=[CH:2][CH:10]=1

参加物

7

実験手順

A solution of 4.1 g of 5-chloro-2-methoxy-benzoyl chloride in 20 ml of toluene was added dropwise to a suspension of 4.65 g of 2-(4-ethylphenyl)-ethylamine hydrochloride in 100 ml of anhydrous toluene after addition of 5 ml of pyridine. The whole was heated under reflux, then shaken with water, dilute hydrochloric acid and a solution of sodium bicarbonate and dried over sodium sulfate. After concentration under reduced pressure, the residue, which solidified only slowly, was filtered off with suction after addition of petroleum ether (B.p. 30°-60° C.). The 5-chloro-2-methoxy-N-(2-<4-ethylphenyl>-ethyl)-benzamide so obtained was found to melt at 66°-68° C.

後処理

  1. temperatureThe whole was heated
  2. temperatureunder reflux
  3. dry with materiala solution of sodium bicarbonate and dried over sodium sulfate
  4. concentrationAfter concentration under reduced pressure
  5. filtrationwas filtered off with suction
  6. additionafter addition of petroleum ether (B.p. 30°-60° C.)

出典と根拠

ORDレコード
ord-8873582cdcbd4096a46fbee0bab7ceb6
出典データセット
uspto-grants-1979_06
特許番号
US04158063

反応ノート

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