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Stannous Chloride → HCID 57494449、化合物

HRID 1260265
ノート
印刷プレビュー

反応式

HRID 1260265 の反応式
[CH2:1]([N:8]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][C:16]([N+:19]([O-])=O)=[C:15]([O:22][CH3:23])[CH:14]=2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Sn](Cl)Cl>CO>[CH2:1]([N:8]1[CH2:12][CH2:11][CH:10]([C:13]2[CH:18]=[CH:17][C:16]([NH2:19])=[C:15]([O:22][CH3:23])[CH:14]=2)[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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 24479Stannous ChlorideHCID 574700891-Benzyl-3-(3-methoxy-4-nitro-phenyl)-pyrrolidine

生成物 1

HCID 57494449HCID 57494449、化合物収率 70%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1-Benzyl-3-(3-methoxy-4-nitro-phenyl)-pyrrolidine (350 mg, 1.12 mmol) was dissolved in methanol (20 ml), tin dichloride (1.912 g, 10.08 mmol) was added, and the reaction mixture stirred at reflux for 2 h. The methanol was evaporated, 1 N sodium hydroxide (50 ml) and ethyl acetate were added and stirring continued. The tin salts were filtered off, the organic phase was separated, dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure to yield an oil (220 mg, 70%).

後処理

  1. temperatureat reflux for 2 h
  2. customThe methanol was evaporated
  3. addition1 N sodium hydroxide (50 ml) and ethyl acetate were added
  4. stirringstirring
  5. filtrationThe tin salts were filtered off
  6. customthe organic phase was separated
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customthe solvent evaporated under reduced pressure

出典と根拠

ORDレコード
ord-48553bec0bad4b84beebc58091c5258a
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08470810B2

反応ノート

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