Sulfuric Acid → HCID 18950694, 화합물

HRID 1492552노트

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HRID 1492552 반응식
O1CCOCC1.CO.C([NH:11][CH:12]([C:25]1[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=1)[CH2:13][CH2:14][C:15]1[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][CH:16]=1)=O.S(=O)(=O)(O)O.C(=O)([O-])O.[Na+]>>[NH2:11][CH:12]([C:25]1[CH:26]=[N:27][CH:28]=[CH:29][CH:30]=1)[CH2:13][CH2:14][C:15]1[CH:24]=[CH:23][C:18]([C:19]([O:21][CH3:22])=[O:20])=[CH:17][CH:16]=1

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 86748334HCID 86748334, 화합물

생성물 1

HCID 18950694HCID 18950694, 화합물수율 87.4%

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온도
60 °C

실험 절차

To 10 ml of the solution of 0.62 g of methyl 4-[3-formamido-3-(3-pyridyl)propyl]benzoate methanol-1,4 dioxane (1:1) was added 5 ml of 4% sulfuric acid, and stirred under heating at 60° C. overnight, which was then poured into saturated aqueous sodium hydrogencarbonate solution to be extracted with ethyl acetate. The obtained ethyl acetate phase was washed in saturated aqueous sodium chloride and dried over magnesium sulfate, to distill off the solvent, so that 0.35 g of methyl 4-[3-amino-3-(3-pyridyl)propyl]benzoate was yielded.

후처리

  1. extractionto be extracted with ethyl acetate
  2. washThe obtained ethyl acetate phase was washed in saturated aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. distillationto distill off the solvent

출처 및 근거

ORD 기록
ord-f3c8f0436cd3406f85d86598960cc551
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05374641

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