Bromine → 3-Bromo-6-(trifluoromethyl)pyridin-2-amine

HRID 451465

反応式

HRID 451465 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[C:7]([NH2:9])[CH:6]=[CH:5][CH:4]=1.[Br:12]Br>ClCCl>[Br:12][C:6]1[C:7]([NH2:9])=[N:8][C:3]([C:2]([F:1])([F:10])[F:11])=[CH:4][CH:5]=1

参加物

4

反応物 2

HCID 24408BromineHCID 8210242-Amino-6-(trifluoromethyl)pyridine

生成物 1

HCID 547588353-Bromo-6-(trifluoromethyl)pyridin-2-amine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 6-(trifluoromethyl)pyridin-2-amine (200 mg, 1.23 mmol) in dichlormethane (2.47 mL) was cooled to 0° C. and bromine (197 mg, 63.4 μL, 1.23 mmol) was slowly added within 30 minutes. After 25 hours at 0° C. the reaction mixture was extracted with saturated Na2S2O3 solution, water and brine, dried over Na2SO4 and concentrated in vacuo. The crude material was purified by flash chromatography over silica gel using CH2Cl2/MeOH (with 10% ammonia) as eluent. The title compound was obtained as a white solid (711 mg, 24%).

後処理

  1. extractionAfter 25 hours at 0° C. the reaction mixture was extracted with saturated Na2S2O3 solution, water and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe crude material was purified by flash chromatography over silica gel

出典と根拠

ORDレコード
ord-f55ec016212748739785ce7fd3b023d5
出典データセット
uspto-grants-2013_07
特許番号
US08486967B2

関連ノート

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