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HRID 25634作成日:2026年10月23日

Pyridine → HCID 178485835、化合物

https://huagongshe.com/ja/reaction/25634

反応式

関与物質

役割名称HCID仕込み量
反応物PyridineHCID 1049—
反応物4-Chlorophenyl IsocyanateHCID 7693—
反応物HCID 178484804HCID 178484804—
溶媒1,4-DioxaneHCID 31275—
溶媒KHSO4 etherHCID 86584777—
生成物HCID 178485835HCID 178485835101.9%

反応手順

A solution of 1.38 g (corresponds to 3.0 mmol) of trans-Methanesulfonic acid 3-(4-methylamino-cyclohexyl)-prop-2-ynyl ester trifluoroacetate in 7 ml dioxane was first cooled to 8° C., treated with 0.69 g (4.5 mmol) 4-chlorophenyl isocyanate and then with 1.2 ml (15 mmol; 5 equivalents) of pyridine (during 3 min). After 45 min at RT, the mixture was dissolved in aqueous 10% KHSO4/Et2O (3×). The organic phases were washed with aqueous 10% NaCl, dried over Na2SO4 and evaporated to give 1.22 g (quantitative) of crude trans-Methanesulfonic acid 3-{4-[3-(4-chloro-phenyl)-1-methyl-ureido]-cyclohexyl}-prop-2-ynyl ester, MS: 398 (MH+, 1Cl). The crude product was directly used in the next step.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06858651B2
出典データセットuspto-grants-2005_02
ORD IDord-28db14751ac646c88829af2b73dfd95f
出典メモuspto-grants-2005_02