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HRID 329927作成日:2026年10月26日

Acetonitrile → 8-(4-(Methylsulfonyl)phenyl)-1,4-dioxa-8-azaspiro[4.5]decane

https://huagongshe.com/reaction/329927

反応式

関与物質

役割名称HCID仕込み量
反応物AcetonitrileHCID 6342—
反応物Potassium CarbonateHCID 11430—
反応物1,4-Dioxa-8-azaspiro(4.5)decaneHCID 67435—
反応物1-Fluoro-4-(methylsulphonyl)benzeneHCID 67994—
溶媒WaterHCID 962—
生成物8-(4-(Methylsulfonyl)phenyl)-1,4-dioxa-8-azaspiro[4.5]decaneHCID 425636077.3%

反応手順

A mixture of 10 g (0.057 mol) of p-fluorophenyl methyl sulfone, 8.72 g (0.063 mol) of K2CO3, 24.66 g (0.172 mol) of 1,4-dioxa-8-azaspiro[4.5]-decane and 50 ml of acetonitrile is stirred overnight at 90°-100° C. After cooling, the mixture is diluted with water and extracted with methylene chloride. The combined extracts are washed with brine, dried over Na2SO4, and concentrated in vacuo. Trituration with ethyl ether affords 13.11 g (77%) of title compound as a white solid: m.p. 192°-194° C.; IR (KBr) 1588, 1369, and 1290 cm-1 ; NMR (CDCl3) δ 7.74 (m, 2H), 6.96 (m, 2H), 4.02 (s, 4H), 3.54 (m, 4H), 3.03 (s, 3H), and 1.81 (m, 4H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04894374
出典データセットuspto-grants-1990_01
ORD IDord-7a0af4ea29a74a42902eadeffd979f2f
出典メモuspto-grants-1990_01