Methanol → Methyl 4-(4-chloro-1-oxobutyl)-alpha,alpha-dimethylbenzeneacetate

HRID 1018090노트

반응식

HRID 1018090 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:18])([CH3:17])[C:14]([OH:16])=[O:15])=[CH:9][CH:8]=1)=[O:6].[CH3:19]O>Cl>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:18])([CH3:17])[C:14]([O:16][CH3:19])=[O:15])=[CH:9][CH:8]=1)=[O:6]

참가 물질

4

반응물 2

HCID 887MethanolHCID 109235672-(4-(4-Chlorobutanoyl)phenyl)-2-methylpropanoic acid

생성물 1

HCID 10062338Methyl 4-(4-chloro-1-oxobutyl)-alpha,alpha-dimethylbenzeneacetate수율 95.1%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매2회

실험 절차

Dissolve 2-[4-(4-chloro-butyryl)-phenyl]-2-methyl-propionic acid (6.2 g, 23.1 mmol) in hot methanolic solution of anhydrous hydrogen chloride (42 mL of a methanol containing 3.2 g of anhydrous hydrogen chloride). Reflux for 42 minutes, evaporate the solvent in vacuo, dissolve the residue in methylene chloride and wash with water. Dry (MgSO4), filter through silica gel, washing the gel with methylene chloride. Combine the organic washings and evaporate the solvent in vacuo to give the title compound as a clear oil (6.21 g, 94%).

후처리

  1. temperatureReflux for 42 minutes
  2. customevaporate the solvent in vacuo
  3. dissolutiondissolve the residue in methylene chloride
  4. washwash with water
  5. dry with materialDry (MgSO4)
  6. filtrationfilter through silica gel
  7. washwashing the gel with methylene chloride
  8. customevaporate the solvent in vacuo

출처 및 근거

ORD 기록
ord-1e180fa813234b39b64a8a367e68485e
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06479663B2

반응 노트

불러오는 중…