Ethyl Acetate → HCID 86647482, 화합물

HRID 2192898노트

반응식

HRID 2192898 반응식
C(OC([NH:8][C:9]1[N:10]=[CH:11][C:12]([CH2:15][C:16]([O:18][CH3:19])=[O:17])=[N:13][CH:14]=1)=O)(C)(C)C.O1CCOCC1.Cl.C(=O)(O)[O-].[Na+].C(OCC)(=O)C>O1CCOCC1.O.[Cl-].[Na+].O>[NH2:8][C:9]1[N:10]=[CH:11][C:12]([CH2:15][C:16]([O:18][CH3:19])=[O:17])=[N:13][CH:14]=1

참가 물질

8

반응물 4

HCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 204431481,4-Dioxane hydrochlorideHCID 86647483HCID 86647483, 화합물

생성물 1

HCID 86647482HCID 86647482, 화합물수율 88.5%

시약·촉매·용매 3

HCID 962Water용매HCID 312751,4-Dioxane용매HCID 57417360Sodium chloride; water용매

실험 절차

To a solution of methyl {5-[(tert-butoxycarbonyl)amino]pyrazin-2-yl}acetate (0.4811 g) in dioxane (5 mL) was added a 4 M hydrogen chloride dioxane solution (5 mL), followed by stirring overnight. The reaction mixture was concentrated and the obtained crude product was collected by filtration and washed with ethyl acetate. The obtained crude product was dissolved in water, and saturated aqueous sodium bicarbonate and ethyl acetate were added thereto, followed by stirring for 1 hour. Saturated brine was added thereto, followed by extraction with ethyl acetate (10 mL×20 times), and the obtained organic layer was washed with saturated brine, dried using anhydrous magnesium sulfate. After concentration under reduced pressure, methyl (5-aminopyrazin-2-yl)acetate (0.2662 g) was obtained as a pale yellow solid.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customthe obtained crude product
  3. filtrationwas collected by filtration
  4. washwashed with ethyl acetate
  5. customThe obtained crude product
  6. stirringby stirring for 1 hour
  7. extractionfollowed by extraction with ethyl acetate (10 mL×20 times)
  8. washthe obtained organic layer was washed with saturated brine
  9. customdried
  10. concentrationAfter concentration under reduced pressure

출처 및 근거

ORD 기록
ord-1252b60c73f64e14bb09a3d193980d5f
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329707B2

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