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

HRID 541479노트

반응식

HRID 541479 반응식
[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]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 68288737Methyl 5-cyano-2,4-dimethylbenzoate2회

생성물 1

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

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-e7399ba79198477495344f4962884360
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871790B2

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