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2-Aminopyridine → 1,2-Diaminopyridin-1-ium 2,4,6-trimethylbenzene-1-sulfonate

HRID 1621169
ノート
印刷プレビュー

反応式

HRID 1621169 の反応式
[C:1]1([CH3:14])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[S:9]([O:12][NH2:13])(=[O:11])=[O:10].[N:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[NH2:21]>ClCCl>[CH3:8][C:3]1[CH:4]=[C:5]([CH3:7])[CH:6]=[C:1]([CH3:14])[C:2]=1[S:9]([O-:12])(=[O:11])=[O:10].[NH2:13][N+:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[NH2:21]
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 104392-AminopyridineHCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine

生成物 1

HCID 122641901,2-Diaminopyridin-1-ium 2,4,6-trimethylbenzene-1-sulfonate収率 82.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of O-(mesitylsulfonyl)hydroxylamine (9.2 g, 42.7 mmol) in dichloromethane (110 mL) was added pyridin-2-amine (4.02 g, 42.7 mmol) in four portions at 0-5° C. to give a yellow solution. After 5 min the yellow solution turned into a light yellow suspension. The ice bath was removed after 10 min and the reaction mixture was stirred at RT for 1 h. The suspension was diluted with diethyl ether (100 mL), filtered, washed with diethyl ether and dried in vacuo to give the product (10.9 g, 35.2 mmol, 82.4%) as light red solid which was used without further purification for the next step.

後処理

  1. customto give a yellow solution
  2. customThe ice bath was removed after 10 min
  3. additionThe suspension was diluted with diethyl ether (100 mL)
  4. filtrationfiltered
  5. washwashed with diethyl ether
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-43e33c7c78274cb99f3f8b054f19d093
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772510B2

反応ノート

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