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HRID 641097作成日:2026年10月26日

Hydrochloric Acid → HCID 178447951、化合物

https://huagongshe.com/reaction/641097

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MagnesiumHCID 5462224—
反応物1-Bromo-2-chloro-4-ethoxy-3-fluorobenzeneHCID 53414983—
反応物HCID 178447952HCID 178447952—
溶媒TolueneHCID 1140—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 178447951HCID 17844795197.8%

反応条件

温度43 °C

反応手順

1.0 g of well dried magnesium and 30 mL of THF were placed in a reactor under nitrogen atmosphere, and heated to 43° C. 10.0 g of 1-bromo-2-chloro-4-ethoxy-3-fluorobenzene (6) dissolved in 20 mL of THF was slowly added dropwise thereto at a temperature range of from 43 to 51° C., followed by stirring for 30 minutes. Thereafter, 21.2 g of 4-(2-(trans-4-propylcyclohexyl)ethyl)cyclohexanone (7) dissolved in 20 mL of THF was slowly added dropwise thereto at a temperature range of from 50 to 55° C., followed by stirring for 30 minutes. After cooling the resulting reaction mixture to 25° C., the reaction mixture was mixed with 100 mL of 3N hydrochloric acid and 100 mL of toluene in a vessel and separated into an organic layer and an aqueous layer by standing still, so as to attain extraction to the organic layer. The resulting organic layer was fractionated and washed with water, a 2N sodium hydroxide aqueous solution, a saturated sodium bicarbonate aqueous solution and water, followed by drying over anhydrous magnesium sulfate. Thereafter, the solvent was removed by distillation under reduced pressure to obtain 16.4 g of 1-(2-chloro-4-ethoxy-3-fluorophenyl)-4-(2-(trans-4-propylcyclohexyl)ethyl)cyclohexanol (8). The resulting compound (8) was a yellow solid matter.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07695777B2
出典データセットuspto-grants-2010_04
ORD IDord-8e7e8d7cef4c431a8ab82706fb466c16
出典メモuspto-grants-2010_04