Diethyl Ether → 1-Amino-2-(3-methoxy-1-propynyl)pyridinium 2,4,6-trimethyl-1-benzenesulfonate

HRID 2253371ノート

反応式

HRID 2253371 の反応式
[CH3:1][O:2][CH2:3][C:4]#[C:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1.[C:12]1([CH3:25])[CH:17]=[C:16]([CH3:18])[CH:15]=[C:14]([CH3:19])[C:13]=1[S:20]([O:23][NH2:24])(=[O:22])=[O:21].C(OCC)C>ClCCl>[CH3:19][C:14]1[CH:15]=[C:16]([CH3:18])[CH:17]=[C:12]([CH3:25])[C:13]=1[S:20]([O-:23])(=[O:22])=[O:21].[NH2:24][N+:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[C:5]#[C:4][CH2:3][O:2][CH3:1]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamineHCID 138648462-(3-Methoxyprop-1-YN-1-YL)pyridine

生成物 1

HCID 230809481-Amino-2-(3-methoxy-1-propynyl)pyridinium 2,4,6-trimethyl-1-benzenesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 2-(3-methoxy-1-propynyl)pyridine (13.2 g) dissolved in dichloromethane (50 mL) was added a solution of O-mesitylenesulfonylhydroxylamine (Reference; Synthesis, 1997, 1) (21 g) in dichloromethane (80 mL) dropwise while cooling with ice, and the reaction mixture was stirred for 30 minutes. Diethyl ether (1 L) was added to the obtained reaction mixture to precipitate crystals, which were collected by filtration and dried under reduced pressure to afford a crude product of 1-amino-2-(3-methoxy-1-propynyl)pyridinium 2,4,6-trimethyl-1-benzenesulfonate as ecru crystals (27.1 g).

後処理

  1. temperaturewhile cooling with 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-aee4daef026f4a79bb12566090f72c42
出典データセット
uspto-grants-2008_01
特許番号
US07323569B2

反応ノート

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