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

HRID 347825

반응식

HRID 347825 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 2-(1-butynyl)pyridine (12.8 g) dissolved in dichloromethane (60 mL) was added a solution of O-mesitylenesulfonylhydroxylamine (Reference; Synthesis, 1997, 1) (20 g) in dichloromethane (132 mL) while cooling with ice, and the reaction mixture was stirred for 30 minutes. Diethyl ether (2 L) was added to the reaction mixture to precipitate crystals, which were filtered off and then dried under reduced pressure to afford a crude product of N-amino-2-(1-butynyl)pyridinium mesitylenesulfonate (12.6 g) as colorless crystals.

후처리

  1. temperaturewhile cooling with ice
  2. customto precipitate crystals, which
  3. filtrationwere filtered off
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-a70a37d229294fbbaa931445ece8feea
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176216B2

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