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

HRID 236089
ノート
印刷プレビュー

反応式

HRID 236089 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-86d6f2488d54497e85f9236dc76824c2
出典データセット
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04642348

反応ノート

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