Water → HCID 86652215、化合物

HRID 217276ノート

反応式

HRID 217276 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 86652215HCID 86652215、化合物収率 77.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-72cca2efee3a4e69b84cf0afdc5b8c6e
出典データセット
uspto-grants-2012_06
特許番号
US08193362B2

反応ノート

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