Hydrochloric Acid → (2S, 4S)-4-(4-Methoxybenzylthio)-2-methoxycarbonylpyrrolidine

HRID 1030144노트

반응식

HRID 1030144 반응식
Cl.C(OC([N:9]1[CH2:13][C@@H:12]([S:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=2)[CH2:11][C@H:10]1[C:24]([O:26][CH3:27])=[O:25])=O)(C)(C)C.C(=O)(O)[O-].[Na+]>C(OCC)(=O)C>[CH3:23][O:22][C:19]1[CH:18]=[CH:17][C:16]([CH2:15][S:14][C@@H:12]2[CH2:13][NH:9][C@H:10]([C:24]([O:26][CH3:27])=[O:25])[CH2:11]2)=[CH:21][CH:20]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 86745654(2S, 4S)-1-(t-butoxycarbonyl)-4-(4-methoxybenzylthio)-2-methoxycarbonylpyrrolidine

생성물 1

HCID 15200411(2S, 4S)-4-(4-Methoxybenzylthio)-2-methoxycarbonylpyrrolidine수율 85.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

27.3 ml of a 4N ethyl acetate solution of hydrogen chloride were added, whilst ice-cooling, to a solution of 5.22 g of (2S, 4S)-1-(t-butoxycarbonyl)-4-(4-methoxybenzylthio)-2-methoxycarbonylpyrrolidine [prepared as described in step (8) above] dissolved in 14 ml of ethyl acetate, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was then poured into a saturated aqueous solution of sodium bicarbonate and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, to give 3.3 g of the title compound as an oil.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with an aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was then removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-c815d4ab07cb4379a9a2295134d918a7
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104867

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