Chlorosuccinimide → 6-Bromo-5-chloropyridin-2-amine

HRID 1521959노트

반응식

HRID 1521959 반응식
[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][CH:3]=1.[Cl:9]N1C(=O)CCC1=O>C(#N)C.C(OCC)(=O)C>[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[Cl:9]

참가 물질

5

반응물 2

HCID 31398ChlorosuccinimideHCID 3008092-Amino-6-bromopyridine

생성물 1

HCID 534011936-Bromo-5-chloropyridin-2-amine

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

To a solution of 6-bromopyridin-2-amine (10 g, 58 mmol) in acetonitrile (150 mL) was added 1-chloropyrrolidine-2,5-dione (8.1 g, 60 mmol) and the mixture was heated at 80° C. for 10 hours. The mixture was diluted with ethyl acetate (200 mL) and washed with water. The organic phase was concentrated and purified by column chromatography (silica gel, 30% ethyl acetate in hexane) to afford the title compound. LCMS: 208 (M+H)+.

후처리

  1. washwashed with water
  2. concentrationThe organic phase was concentrated
  3. custompurified by column chromatography (silica gel, 30% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-96a9d554444142d3b6f9b07200c100d2
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073922B2

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