Methanesulfonic Acid → HCID 67548859, 화합물

HRID 43736노트

반응식

HRID 43736 반응식
CS(O)(=O)=O.[CH:6]([O:9][CH:10]1[C:15](OC)([O:16]C)[CH2:14][CH2:13][N:12]([C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])[CH2:11]1)([CH3:8])[CH3:7].C(=O)(O)[O-].[Na+]>CC(C)=O>[CH:6]([O:9][CH:10]1[C:15](=[O:16])[CH2:14][CH2:13][N:12]([C:20]([O:22][C:23]([CH3:25])([CH3:24])[CH3:26])=[O:21])[CH2:11]1)([CH3:8])[CH3:7]

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 516892Sodium BicarbonateHCID 67549716tert-Butyl 3-isopropoxy-4,4-dimethoxypiperidine-1-carboxylate

생성물 1

HCID 67548859HCID 67548859, 화합물수율 52.8%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Methanesulfonic acid (0.8 mL) was added to a solution of tert-butyl 3-isopropoxy-4,4-dimethoxypiperidine-1-carboxylate obtained in Example (147b) (248 mg, 0.817 mmol) in acetone (3 mL). The mixture was stirred at room temperature overnight and further stirred at 50° C. for 35 minutes. Following cooling, saturated aqueous sodium bicarbonate solution was added to the reaction solution, and the organic substance was extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, and then the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate) to obtain 111 mg of the title compound as a colorless oily substance (53%).

후처리

  1. stirringfurther stirred at 50° C. for 35 minutes
  2. temperatureFollowing cooling
  3. extractionthe organic substance was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-8a9737661dc443478ca364032b17f5be
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536197B2

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