Hydrochloric Acid → HCID 64993550, 화합물

HRID 1774571노트

반응식

HRID 1774571 반응식
C([C:4]1[N:5]=[CH:6][S:7][CH:8]=1)(=O)C.[CH3:9][O:10][CH:11]([O:16][CH3:17])[C:12]([O:14]C)=O.[CH3:18][O-:19].[Na+].[CH3:21]O.Cl>C(OCC)C.C(OCC)(=O)C.O>[CH3:17][O:16][CH:11]([O:10][CH3:9])[C:12](=[O:14])[CH2:21][C:18]([C:6]1[S:7][CH:8]=[CH:4][N:5]=1)=[O:19]

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 887MethanolHCID 66647Acetic acid, 2,2-dimethoxy-, methyl esterHCID 33480311-(Thiazol-4-yl)ethanoneHCID 10942334Sodium Methoxide

생성물 1

HCID 64993550HCID 64993550, 화합물수율 88%

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 4-acetylthiazole (1.0 g, 7.86 mmol) and methyl dimethoxyacetate (1.05 g, 7.86 mmol) in anhydrous diethyl ether (15 mL) was treated with sodium methoxide 4.37M in methanol (1.80 mL, 7.86 mmol) at 0° C. The resulting mixture was stirred at room temperature for 3 hours, and then diluted with ethyl acetate (10 mL). After cooling to 0° C., the reaction mixture was neutralized with 1N hydrochloric acid until pH 3 was reached. Water was added (6 mL) and layers were separated. The organic layer was washed with brine (10 mL), dried over sodium sulfate and concentrated in vacuo to provide 4,4-dimethoxy-1-(1,3-thiazol-2-yl)butane-1,3-dione (8a) (1.58 g, 6.89 mmol, 88%) which was used without further purification.

후처리

  1. temperatureAfter cooling to 0° C.
  2. customwere separated
  3. washThe organic layer was washed with brine (10 mL)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-6377240c0a0f41ee8c234cd5e52110bb
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09260395B2

반응 노트

불러오는 중…