戻る
化工社化工社 化学情報印刷レポート · 研究参考用
HRID 632552作成日:2026年10月24日

Diethyl Ether → HCID 58360463、化合物

https://huagongshe.com/ja/reaction/632552

反応式

関与物質

役割名称HCID仕込み量
反応物Diethyl EtherHCID 3283—
反応物Sodium hydrideHCID 24758—
反応物Trimethyloxosulphonium chlorideHCID 197819—
反応物HCID 58114000HCID 58114000—
溶媒Dimethyl SulfoxideHCID 679—
溶媒TetrahydrofuranHCID 8028—
溶媒Sodium chloride; waterHCID 57417360—
生成物HCID 58360463HCID 5836046337%

反応手順

NaH (140 mg of a 60% oil dispersion, 3.50 mmol) was added in portions to a solution of trimethylsulfoxonium chloride (452 mg, 3.51 mmol) in DMSO (8.0 mL) at room temperature. After 15 min, a solution of 5-(3,3-dimethyl-but-1-ynyl)-3-[(4-methyl-cyclohexanecarbonyl)-(4-oxo-cyclohexyl)-amino]-thiophene-2-carboxylic acid methyl ester (1.34 g, 2.93 mmol) in THF (8.0 mL) was added dropwise. After 3 h, brine was added and the reaction extracted with ethyl acetate. The combined organic layers were washed with water, brine, dried over Na2SO4 and concentrated to give a viscous yellow oil. Trituration with ethyl ether and hexanes provided 5-(3,3-dimethyl-but-1-ynyl)-3-[(4-methyl-cyclohexanecarbonyl)-(1-oxa-spiro[2.5]oct-6-yl)-amino]-thiophene-2-carboxylic acid methyl ester (509 mg, 37%) as a colorless solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09321753B2
出典データセットuspto-grants-2016_04
ORD IDord-136b43c6c0984e44ac86f81e455a481a
出典メモuspto-grants-2016_04