Potassium Carbonate → 9-bromo-6-(4-methoxybenzyl)pyrido[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5(6H)-one

HRID 707472

反応式

HRID 707472 の反応式
Cl[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[CH:5][CH:4]=1.[Br:11][C:12]1[CH:21]=[N:20][C:19]2[NH:18][C:17](=[O:22])[N:16]3[N:23]=[CH:24][N:25]=[C:15]3[C:14]=2[CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>CN1CCCC1=O>[Br:11][C:12]1[CH:21]=[N:20][C:19]2[N:18]([CH2:2][C:3]3[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[CH:5][CH:4]=3)[C:17](=[O:22])[N:16]3[N:23]=[CH:24][N:25]=[C:15]3[C:14]=2[CH:13]=1

参加物

5

反応条件

温度
40 °C

実験手順

1-(Chloromethyl)-4-methoxybenzene (3.10 ml, 22.9 mmol) was added to a stirred solution of 9-bromopyrido[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5(6H)-one (3.02 g, 11.35 mmol) and potassium carbonate (4.71 g, 34.1 mmol) in 1-methylpyrrolidinone (60 ml) and the mixture was heated at 40° C. for 14 hours. The mixture was filtered, and the resulting solid was washed liberally with dichloromethane. The combined organics were concentrated under vacuum and the residue was triturated with ethyl acetate (40 mL) to afford 3.07 g (70%) of the benzylated product as a brown powder.

後処理

  1. filtrationThe mixture was filtered
  2. washthe resulting solid was washed liberally with dichloromethane
  3. concentrationThe combined organics were concentrated under vacuum
  4. customthe residue was triturated with ethyl acetate (40 mL)

出典と根拠

ORDレコード
ord-9f1f0f00d6fc48258b45a252c5d7ad14
出典データセット
uspto-grants-2015_11
特許番号
US09175010B2

関連ノート

読み込み中…