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HRID 268118作成日:2026年10月27日

Resorcinol → 1,2-Dihydro-9-hydroxy-1-methyl-7-(3-methyl-2-octyl)-4-oxo4H-thieno-[2,3-c][1] benzopyran

https://huagongshe.com/reaction/268118

反応式

関与物質

役割名称HCID仕込み量
反応物ResorcinolHCID 5054—
反応物Phosphorus oxychlorideHCID 24813—
反応物5-(3-Methyloctan-2-yl)benzene-1,3-diolHCID 258176—
反応物Methyl tetrahydro-4-methyl-3-oxo-2-thiophenecarboxylateHCID 10487456—
溶媒BenzeneHCID 241—
生成物1,2-Dihydro-9-hydroxy-1-methyl-7-(3-methyl-2-octyl)-4-oxo4H-thieno-[2,3-c][1] benzopyranHCID 21519990—

反応手順

A solution in dry benzene of equimolar amounts of methyl 4-methyl-3-oxo-tetrahydrothiophene-2-carboxylate and 5-(3-methyl-2-octyl) resorcinol plus phosphorous oxychloride (5 ml. of benzene/g. of the resorcinol) was warmed for 13 days at 35°-37°C. in an oil bath. Most of the benzene and HCl were removed at reduced pressure, and the dark tarry residue was stirred with ether and water until solution was complete. The ether layer was washed successively with dilute solutions of sodium bicarbonate, sodium hydroxide and sodium carbonate, then with water and saturated sodium chloride. Drying and concentrating the final organic solution left a friable brick-red foamy solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US03946111
出典データセットuspto-grants-1976_03
ORD IDord-a079d58fdd594ec28413d3cb891bd874
出典メモuspto-grants-1976_03