Diethyl Ether → N-amino-2-(1-butynyl)pyridinium mesitylenesulfonate

HRID 1181856

反応式

HRID 1181856 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][N:6]=1)#[C:2][CH2:3][CH3:4].[C:11]1([CH3:24])[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]([CH3:18])[C:12]=1[S:19]([O:22][NH2:23])(=[O:21])=[O:20].C(OCC)C>ClCCl>[C:11]1([CH3:24])[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]([CH3:18])[C:12]=1[S:19]([O-:22])(=[O:21])=[O:20].[NH2:23][N+:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[C:1]#[C:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamineHCID 212993912-(1-Butynyl)pyridine

生成物 1

HCID 21984654N-amino-2-(1-butynyl)pyridinium mesitylenesulfonate収率 39.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

After dissolving 2-(1-butynyl)pyridine (12.8 g) in dichloromethane (60 mL), a solution of O-mesitylenesulfonylhydroxyamine (Reference document: Synthesis, 1997, 1) (20 g) in dichloromethane (132 mL) was added dropwise while cooling on ice, and the mixture was stirred for 30 minutes. Diethyl ether (2 L) was added to the reaction mixture to precipitate crystals, which were collected by filtration and dried under reduced pressure to obtain N-amino-2-(1-butynyl)pyridinium mesitylenesulfonate (12.6 g) as colorless crystals.

後処理

  1. temperaturewhile cooling on ice
  2. customto precipitate crystals, which
  3. filtrationwere collected by filtration
  4. customdried under reduced pressure

出典と根拠

ORDレコード
ord-1c821463d979462c976f1df19d67d338
出典データセット
uspto-grants-2007_10
特許番号
US07285666B2

関連ノート

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