Hydrochloric Acid → Methyl 5-(imino(methoxy)methyl)-2,4-dimethylbenzoate hydrochloride

HRID 541479ノート

反応式

HRID 541479 の反応式
[C:1]([C:3]1[C:4]([CH3:14])=[CH:5][C:6]([CH3:13])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9])#[N:2].[ClH:15].[CH3:16][OH:17]>>[ClH:15].[NH:2]=[C:1]([O:17][CH3:16])[C:3]1[C:4]([CH3:14])=[CH:5][C:6]([CH3:13])=[C:7]([CH:12]=1)[C:8]([O:10][CH3:11])=[O:9]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 68288737Methyl 5-cyano-2,4-dimethylbenzoate2 回

生成物 1

HCID 68288394Methyl 5-(imino(methoxy)methyl)-2,4-dimethylbenzoate hydrochloride収率 15%

実験手順

Into a 50-mL three neck round-bottom flask, was placed a solution of methyl 5-cyano-2,4-dimethylbenzoate (compound 2.3, 900 mg, 4.28 mmol, 1.00 equiv, 90%) in methanol (20 mL). Hydrogen chloride gas was introduced by bubbling through the solution for 0.5 hr. The reaction mixture was then transferred into a 30-mL sealed tube and stirred overnight at room temperature. The mixture was concentrated under vacuum and the residue was diluted with ethyl acetate (30 mL) and extracted with water (10 mL). The aqueous was concentrated in vacuo to obtain the title compound as a white solid (200 mg, 15%).

後処理

  1. customby bubbling through the solution for 0.5 hr
  2. customsealed tube
  3. concentrationThe mixture was concentrated under vacuum
  4. additionthe residue was diluted with ethyl acetate (30 mL)
  5. extractionextracted with water (10 mL)
  6. concentrationThe aqueous was concentrated in vacuo

出典と根拠

ORDレコード
ord-e7399ba79198477495344f4962884360
出典データセット
uspto-grants-2014_10
特許番号
US08871790B2

反応ノート

読み込み中…