Tetramethoxypropane → 2-(5-Bromopyridin-3-yl)pyrimidine

HRID 50576

反応式

HRID 50576 の反応式
[C:1]([C:4]1[CH:5]=[N:6][CH:7]=[C:8]([Br:10])[CH:9]=1)(=[NH:3])[NH2:2].CO[CH:13](OC)[CH2:14][CH:15](OC)OC>CN(C=O)C>[Br:10][C:8]1[CH:7]=[N:6][CH:5]=[C:4]([C:1]2[N:2]=[CH:15][CH:14]=[CH:13][N:3]=2)[CH:9]=1

参加物

4

反応物 2

HCID 66019TetramethoxypropaneHCID 227351825-Bromonicotinimidamide

生成物 1

HCID 227351782-(5-Bromopyridin-3-yl)pyrimidine収率 22%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

A mixture of the product of Step B (4.86 g, 20.5 mmol) and 1,1,3,3-tetramethoxypropane (6.59 mL, 40 mmol) in DMF (25 mL) was warmed to 90° C. under N2. After 18 h, the reaction mixture was allowed to cool to 25° C., concentrated in vacuo. Purification of the residue by flash chromatography (EtOAc) afforded the title compound (1.05 g, 22%) as a white solid. MS 237 (M+H)+

後処理

  1. temperatureto cool to 25° C.
  2. concentrationconcentrated in vacuo
  3. customPurification of the residue by flash chromatography (EtOAc)

出典と根拠

ORDレコード
ord-7965c9f22cdb4c98b630f5880c75baee
出典データセット
uspto-grants-2004_03
特許番号
US06713455B2

関連ノート

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