Triethylamine → 2-chloro-N-cyclopropyl-5-fluoropyrimidin-4-amine

HRID 2400334ノート

反応式

HRID 2400334 の反応式
[Cl:1][C:2]1C=[C:6](Cl)[C:5]([F:9])=[CH:4][N:3]=1.CC[N:12](CC)CC.[CH:17]1([NH2:20])[CH2:19][CH2:18]1>CC#N>[Cl:1][C:2]1[N:12]=[C:6]([NH:20][CH:17]2[CH2:19][CH2:18]2)[C:5]([F:9])=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 69828CyclopropylamineHCID 220610192,4-Dichloro-5-fluoropyridine

生成物 1

HCID 53067942-chloro-N-cyclopropyl-5-fluoropyrimidin-4-amine収率 81.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

反応条件

温度
0 °C

実験手順

To 2,4 dichloro-5-fluoropyridine (1 g, 6 mmol) dissolved in CH3CN (8 ml) cooled in an ice bath was added Et3N (1.16 ml, 8.4 mmol) and cyclopropylamine (0.29 ml, 8.4 mmol) in CH3CN (2 ml). Reaction stirred 0° C. for 2 hours, evaporated water added and reaction extracted with EtOAc (×3). The organic fractions were combined washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure to give the product (0.92 g).

後処理

  1. temperaturecooled in an ice bath
  2. customReaction
  3. customevaporated water
  4. additionadded
  5. customreaction
  6. extractionextracted with EtOAc (×3)
  7. washThe organic fractions were combined washed with brine
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-5e0cb507574b4ece835653e28df8ff43
出典データセット
uspto-grants-2014_08
特許番号
US08796244B2

反応ノート

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