Hydrochloride methanol → 4-(6-aminopyridin-2-yl)-N-methylbenzenesulfonamide hydrochloride

HRID 17971

反応式

HRID 17971 の反応式
[CH3:1][NH:2][S:3]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:17]=[C:16]([NH:18]C(=O)OC(C)(C)C)[CH:15]=[CH:14][CH:13]=2)=[CH:8][CH:7]=1)(=[O:5])=[O:4].[ClH:26].CO>CO>[ClH:26].[NH2:18][C:16]1[N:17]=[C:12]([C:9]2[CH:10]=[CH:11][C:6]([S:3]([NH:2][CH3:1])(=[O:4])=[O:5])=[CH:7][CH:8]=2)[CH:13]=[CH:14][CH:15]=1

参加物

4

反応物 2

HCID 21893726Hydrochloride methanolHCID 59166177tert-butyl 6-(4-(N-methylsulfamoyl)phenyl)pyridin-2-ylcarbamate

生成物 1

HCID 671338694-(6-aminopyridin-2-yl)-N-methylbenzenesulfonamide hydrochloride収率 71%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of tert-butyl 6-(4-(N-methylsulfamoyl)phenyl)pyridin-2-ylcarbamate (8.5 g, 23.4 mmol) in MeOH (10 mL) was added HCl/MeOH (2M, 50 mL) at room temperature. The suspension was stirred at room temperature overnight. The solid product was collected by filtration, washed with MeOH, and dried to give 4-(6-aminopyridin-2-yl)-N-methylbenzenesulfonamide hydrochloride (5.0 g, 71%). 1H NMR (300 Hz, DMSO-d6) δ 8.12 (d, J=8.4 Hz, 2H), 7.91-7.96 (m, 3H), 7.58-7.66 (m, 1H), 7.31-7.53 (m, 1H), 7.27 (d, J=6.6, 1H), 6.97 (d, J=9.0, 1H), 2.43 (d, J=4.8 Hz, 3H). MS (ESI) m/z (M+H)+ 264.0.

後処理

  1. filtrationThe solid product was collected by filtration
  2. washwashed with MeOH
  3. customdried

出典と根拠

ORDレコード
ord-7349bd6e887b4576876388ab6d866fc3
出典データセット
uspto-grants-2010_06
特許番号
US07741321B2

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