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

HRID 1621169
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인쇄 미리보기

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HRID 1621169 반응식
[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]
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참가 물질

4

반응물 2

HCID 104392-AminopyridineHCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-43e33c7c78274cb99f3f8b054f19d093
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772510B2

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