Sulfuryl chloride → 5-Bromo-2-chloro-1,3-benzothiazole

反応式

S(Cl)([Cl:4])(=O)=O.[Br:6][C:7]1[CH:8]=[CH:9][C:10]2[S:14][C:13](S)=[N:12][C:11]=2[CH:16]=1>>[Br:6][C:7]1[CH:8]=[CH:9][C:10]2[S:14][C:13]([Cl:4])=[N:12][C:11]=2[CH:16]=1

参加物

反応物 2

HCID 24648Sulfuryl chloride

HCID 178527757HCID 178527757、化合物

生成物 1

HCID 202512695-Bromo-2-chloro-1,3-benzothiazole収率 100%

実験手順

To sulfuryl dichloride (5 mL) was added 5-bromobenzo[d]thiazole-2-thiol (450 mg, 1.8 mmol) portionwise. The mixture was stirred at rt for 1 hour and heated at 50° C. for 15 min. After cooling to rt, the reaction mixture was slowly poured onto ice (50 g) and the resulting suspension was stirred for 30 min. Solid was collected through filtration and washed with water (10 mL) and dried under high vacuum to afford 5-bromo-2-chlorobenzo[d]thiazole as a pink solid (470 mg, 100%). MS (ESI) m/z 248 (M+H+).

後処理

temperatureheated at 50° C. for 15 min
temperatureAfter cooling to rt
additionthe reaction mixture was slowly poured onto ice (50 g)
stirringthe resulting suspension was stirred for 30 min
filtrationSolid was collected through filtration
washwashed with water (10 mL)
customdried under high vacuum

出典と根拠

ORDレコード: ord-28443ae781844559a83c7081fbfc3abf
出典データセット: uspto-grants-2013_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08420052B2

反応ノート

読み込み中…

参加物