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HRID 1004122作成日:2026年10月27日

Hydrochloric Acid → Ethyl (E)-3-[5,6-dimethoxy-3-(4-methoxyphenoxy)-benzo[b]thiophen-2-yl]-propenoat

https://huagongshe.com/reaction/1004122

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物(Ethoxycarbonylmethyl)triphenylphosphonium bromideHCID 73731—
反応物5,6-Dimethoxy-3-(4-methoxyphenoxy)benzo[b]thiophene-2-carbaldehydeHCID 11089215—
反応物Potassium tert-butoxideHCID 23665647—
溶媒TetrahydrofuranHCID 8028—
生成物Ethyl (E)-3-[5,6-dimethoxy-3-(4-methoxyphenoxy)-benzo[b]thiophen-2-yl]-propenoatHCID 9888011—

反応手順

20 ml of a 1M solution of potassium tert-butylate in tetrahydrofuran are added dropwise at 0° C. under an inert atmosphere to a suspension of 0.02 mol of (ethoxycarbonylmethyl)triphenylphosphonium bromide in 90 ml of tetrahydrofuran. After the addition is complete and the mixture has returned to room temperature, 0.01 mol of the compound obtained in Step E of Example 1 diluted in 30 ml of tetrahydrofuran is added. After 12 hours, the reaction mixture is hydrolysed by the addition of 100 ml of a 1N HCl solution, and then extracted with ethyl acetate; the combined organic phases are washed with water and then with a saturated NaCl solution, dried over sodium sulphate, filtered and concentrated under reduced pressure. Chromatography over silica gel (pentane/ethyl acetate: 90/10) enables 2.78 g of the expected product to be isolated.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06048875
出典データセットuspto-grants-2000_04
ORD IDord-c2c30a8897d44b19871b8e822c77a7bb
出典メモuspto-grants-2000_04