Allylamine → N-2-Propen-1-yl-6-[4-(trifluoromethyl)phenyl]-2-pyridinamine

HRID 1269670ノート

反応式

HRID 1269670 の反応式
[CH2:1]([NH2:4])[CH:2]=[CH2:3].Br[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][CH:13]=2)[N:7]=1>C(O)C.S([O-])([O-])(=O)=O.[Cu+2]>[CH2:1]([NH:4][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:19])([F:21])[F:20])=[CH:14][CH:13]=2)[N:7]=1)[CH:2]=[CH2:3]

参加物

5

反応物 2

HCID 7853AllylamineHCID 184483252-Bromo-6-(4-(trifluoromethyl)phenyl)pyridine

生成物 1

HCID 18448421N-2-Propen-1-yl-6-[4-(trifluoromethyl)phenyl]-2-pyridinamine収率 74.8%

試薬・触媒・溶媒 2

HCID 24462Copper Sulfate触媒HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

A mixture of of allylamine (0.447 mL, 5.96 mmol) and 2-bromo-6-[4-(trifluoromethyl)phenyl]pyridine (0.1 g, 0.298 mmol) in ethanol (5 mL) were heated at 100° C. in a 25 mL pressure vessel. After heating overnight the reaction was cooled and copper sulfate was added and heating continued at 100° C. overnight. After this time the reaction was allowed to coole to room temperature and concentrated in vacuo. Purification by SPE (Silica, 10 g) eluting 3:1 cyclohexane:chloroform afforded the title compound as a dark yellow solid (0.062 g).

後処理

  1. temperatureAfter heating overnight the reaction
  2. temperaturewas cooled
  3. temperatureheating
  4. customto coole to room temperature
  5. concentrationconcentrated in vacuo
  6. customPurification by SPE (Silica, 10 g)
  7. washeluting 3:1 cyclohexane

出典と根拠

ORDレコード
ord-546d2e7ec73a4f6e9519db19b5087601
出典データセット
uspto-grants-2007_04
特許番号
US07199239B2

反応ノート

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