Tin chloride monohydrate → 2-amino-N-(4-chloropyridin-3-yl)benzamide hydrochloride

HRID 44240

反応式

HRID 44240 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][C:3]=1[NH:8][C:9](=[O:19])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[N+:16]([O-])=O.O.[Sn](Cl)(Cl)(Cl)Cl>O1CCOCC1>[ClH:1].[NH2:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[C:9]([NH:8][C:3]1[CH:4]=[N:5][CH:6]=[CH:7][C:2]=1[Cl:1])=[O:19]

参加物

4

反応物 2

HCID 45051637Tin chloride monohydrateHCID 67434091N-(4-chloropyridin-3-yl)-2-nitrobenzamide

生成物 1

HCID 674339602-amino-N-(4-chloropyridin-3-yl)benzamide hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
90 °C

実験手順

A suspension of N-(4-chloropyridin-3-yl)-2-nitrobenzamide (1.9 g, 6.8 mmol) in dioxane (10 mL) and conc. HCL (40 mL) was treated with tin chloride hydrate (6.2 g, 27.2 mmol). The reaction mixture was stirred at 90° C. for one hour (the mixture evolved from suspension to solution and back to suspension). After cooling down, the precipitate was filtered off and dried under high vacuum. The 2-amino-N-(4-chloropyridin-3-yl)benzamide hydrochloride was obtained as an off-white solid (3.0 g). LCMS [M+H]: 248.

後処理

  1. temperatureAfter cooling down
  2. filtrationthe precipitate was filtered off
  3. customdried under high vacuum

出典と根拠

ORDレコード
ord-0410ad2bfead440595a292cfa64d8044
出典データセット
uspto-grants-2013_09
特許番号
US08541407B2

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