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Sodium Methoxide → 3-[(4-Methoxyphenyl)sulfonyl]pyrrolidine hydrochloride

HRID 1981787
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반응식

HRID 1981787 반응식
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([CH:12]2[CH2:16][CH2:15][NH:14][CH2:13]2)(=[O:11])=[O:10])=[CH:5][CH:4]=1.[CH3:17][O-:18].[Na+]>CS(C)=O>[ClH:2].[CH3:17][O:18][C:3]1[CH:8]=[CH:7][C:6]([S:9]([CH:12]2[CH2:16][CH2:15][NH:14][CH2:13]2)(=[O:11])=[O:10])=[CH:5][CH:4]=1
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참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 202178543-((4-Chlorophenyl)sulfonyl)pyrrolidine hydrochloride

생성물 1

HCID 202178603-[(4-Methoxyphenyl)sulfonyl]pyrrolidine hydrochloride

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A solution of 15.5 g (0.060 mole) of 3-[(4-chlorophenyl)sulfonyl]pyrrolidine hydrochloride and 9.0 g (0.167 mole) of sodium methoxide in 200 ml of dimethylsulfoxide was stirred at 100° C. for 2 hours. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and water. The methylene chloride solution was dried over magnesium sulfate and the solvent was removed in vacuo to give an oil, the free base of the title compound. The hydrochloride salt was prepared, recrystallizing from methanol-diethyl ether to give 9.1 g (55%) of white crystalline solid, m.p. 181°-182° C.

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residue was partitioned between methylene chloride and water
  3. dry with materialThe methylene chloride solution was dried over magnesium sulfate
  4. customthe solvent was removed in vacuo
  5. customto give an oil

출처 및 근거

ORD 기록
ord-e060989cff4c461e97228f05095f9e7c
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04593102

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