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HRID 1871213作成日:2026年10月23日

Bromine → 6-Bromo-3,4-dihydro-4,4,5,8-tetramethyl-2H-1-benzothiopyran

https://huagongshe.com/ja/reaction/1871213

反応式

関与物質

役割名称HCID仕込み量
反応物BromineHCID 24408—
反応物4,4,5,8-TetramethylthiochromanHCID 12993684—
反応物Sodium BisulfiteHCID 23665763—
溶媒DichloromethaneHCID 6344—
生成物6-Bromo-3,4-dihydro-4,4,5,8-tetramethyl-2H-1-benzothiopyranHCID 1299368587.1%

反応手順

100 ml of methylene chloride was added to 13.2 g (0.064 mol) of 4,4,5,8-tetramethylthiochroman, 10.2 g (0.064 mol) of bromine was dropwise added at room temperature, and then the mixture was allowed to react for 2 hours. After the completion of the reaction, 70 ml of a 2% sodium hydrogensulfite aqueous solution was added, excessive bromine was removed, and the reaction mixture was liquid-separated. An organic layer was washed with a saturated sodium hydrogencarbonate aqueous solution and with a saturated sodium chloride aqueous solution, and dried over anhydrous sodium sulfate. The methylene chloride was distilled off under reduced pressure, and the resultant oily substance was purified by silica gel column chromatography to give 15.9 g (yield 87%) of 4,4,5,8-tetramethyl-6-bromothiochroman.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06103668
出典データセットuspto-grants-2000_08
ORD IDord-ee664f1fd4704d80b217e11afca7539b
出典メモuspto-grants-2000_08