Methanol → HCID 67453617、化合物

HRID 1474085ノート

反応式

HRID 1474085 の反応式
[Na].F[C:3]1[N:8]=[C:7]([C:9]2([C:13]#[N:14])[CH2:12][CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=1.[CH3:15][OH:16]>>[CH3:15][O:16][C:3]1[N:8]=[C:7]([C:9]2([C:13]#[N:14])[CH2:12][CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=1

参加物

4

反応物 3

HCID 887MethanolHCID 5360545SodiumHCID 67452252HCID 67452252、化合物

生成物 1

HCID 67453617HCID 67453617、化合物収率 97%

反応条件

温度
75 °C

実験手順

To anhydrous methanol (6.0 mL) at 0° C. under nitrogen was added sodium metal (˜1 g) and the mixture stirred for 30 minutes. To the reaction mixture was added 1-(6-fluoropyridin-2-yl)cyclobutanecarbonitrile (1.6 g, 9.1 mmol) followed by heating to 75° C. and stirring for 45 minutes. The solution was cooled to room temperature and partitioned between water and EtOAc. The layers were separated, the aqueous phase was extracted with EtOAc, and the combined organic phases were washed with saturated NaCl, dried over Na2SO4, and concentrated in vacuo to give the desired product (1.7 g, 97%) as a colorless oil.

後処理

  1. stirringstirring for 45 minutes
  2. temperatureThe solution was cooled to room temperature
  3. custompartitioned between water and EtOAc
  4. customThe layers were separated
  5. extractionthe aqueous phase was extracted with EtOAc
  6. washthe combined organic phases were washed with saturated NaCl
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-57a2c1aae25a411ebf83bb8807253340
出典データセット
uspto-grants-2015_04
特許番号
US09018223B2

反応ノート

読み込み中…