Sulfuric Acid → HCID 54289398, 화합물

HRID 566120노트

반응식

HRID 566120 반응식
S([O-])([O-])(=O)=O.[Mg+2].S(=O)(=O)(O)O.[CH2:12]([O:19][C:20]([CH:22]([NH:28][CH3:29])[CH2:23][CH2:24][C:25]([OH:27])=[O:26])=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(=O)([O-])O.[Na+]>C(O)(C)(C)C.ClCCl>[CH2:12]([O:19][C:20]([CH:22]([NH:28][CH3:29])[CH2:23][CH2:24][C:25]([O:27][C:13]([CH3:18])([CH3:14])[CH3:12])=[O:26])=[O:21])[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 24083Sulfuric acid magnesium salt (1:1)2회HCID 516892Sodium BicarbonateHCID 18472650HCID 18472650, 화합물

생성물 1

HCID 54289398HCID 54289398, 화합물수율 106.9%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6386tert-Butanol용매

실험 절차

To dichloromethane (1000 ml) was added at room temperature anhydrous magnesium sulfate (50.6 g) and then concentrated sulfuric acid (6.0 ml). The mixture was stirred at room temperature for 15 minutes, and to the mixture was added 4-[(benzyloxy)carbonyl]-4-methylaminobutyric acid (26.3 g) and then tert-butanol (50.5 ml). The mixture was sealed completely and stirred at room temperature for 18 hours. To the mixture was added saturated sodium hydrogen carbonate solution to dissolve all of the magnesium sulfate, and the mixture was stirred. The organic layer was separated, washed with saturated brine (400 ml) and dried with anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified with silica gel column chromatography (250 g, hexane:ethyl acetate=5:1) to give tert-butyl 4-[(benzyloxy)-carbonyl]-4-methylaminobutyrate (17.2 g, 53%).

후처리

  1. customThe mixture was sealed completely
  2. stirringstirred at room temperature for 18 hours
  3. stirringthe mixture was stirred
  4. customThe organic layer was separated
  5. washwashed with saturated brine (400 ml)
  6. dry with materialdried with anhydrous magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. customthe residue was purified with silica gel column chromatography (250 g, hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-af2ad7451c284ffd86c88f76e23dc0f8
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06172061B2

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