Water → HCID 86652215, 화합물

HRID 1896631노트

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HRID 1896631 반응식
[F:1][CH:2]([F:10])[C:3]1[N:8]=[CH:7][C:6]([NH2:9])=[CH:5][CH:4]=1.[Br:11]N1C(=O)CCC1=O.O>C(#N)C>[Br:11][C:7]1[C:6]([NH2:9])=[CH:5][CH:4]=[C:3]([CH:2]([F:10])[F:1])[N:8]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 552816746-(Difluoromethyl)pyridin-3-amine

생성물 1

HCID 86652215HCID 86652215, 화합물수율 77.9%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of the compound obtained in Step D (2.1 g) and N-bromo-succinimide (2.56 g) in acetonitrile (50 ml) was stirred at 0° C. for 10 minutes. The reaction mixture was poured into water and extracted several times with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate and then concentrated in vacuo. Chromatography on silica gel (eluent: hexane/ethyl acetate 1:1) afforded 2-bromo-6-difluoromethyl-pyridin-3-yl-amine (2.5 g) as a solid. MS (ES+) 223/225 (MH+); 1H NMR (400 MHz, CDCl3) 4.38 (br s, 2H), 6.52 (t, 1H), 7.08 (d, 1H), 7.41 (d, 1H).

후처리

  1. extractionextracted several times with ethyl acetate
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f2bec67cad034b6bbd54a5458fe456fe
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518971B2

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