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

HRID 44240

반응식

HRID 44240 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0410ad2bfead440595a292cfa64d8044
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541407B2

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