Phosphorus oxychloride → 3-Bromo-4-chloro-7-methylthieno[3,2-c]pyridine

反応式

[Br:1][C:2]1[C:6]2[C:7](=O)[NH:8][CH:9]=[C:10]([CH3:11])[C:5]=2[S:4][CH:3]=1.O=P(Cl)(Cl)[Cl:15]>>[Br:1][C:2]1[C:6]2[C:7]([Cl:15])=[N:8][CH:9]=[C:10]([CH3:11])[C:5]=2[S:4][CH:3]=1

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 184507923-Bromo-7-methylthieno[3,2-c]pyridin-4(5h)-one

生成物 1

HCID 184507713-Bromo-4-chloro-7-methylthieno[3,2-c]pyridine収率 64%

実験手順

A solution of Example 277B (10,25 g, 42.1 mmol) in POCl3 (50 mL) was stirred at reflux for 2 hours, cooled to room temperature, diluted with ice water, and stirred vigorously resulting in a precipitate which was collected by filtration. The filter cake was further purified by silica gel chromatography on silica gel with dichloromethane to provide 7.14 g (64% yield) of the desired product. MS (ESI(+)) m/e 261.9, 263.9 (M+H)+.

後処理

temperatureat reflux for 2 hours
customresulting in a precipitate which
filtrationwas collected by filtration
customThe filter cake was further purified by silica gel chromatography on silica gel with dichloromethane

出典と根拠

ORDレコード: ord-29a8ba481ba240018a7641e723793f50
出典データセット: uspto-grants-2010_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07737160B2

反応ノート

読み込み中…

参加物