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Pyridine → HCID 178485835、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-Chlorophenyl Isocyanate | HCID 7693 | — |
| 反応物 | HCID 178484804 | HCID 178484804 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 溶媒 | KHSO4 ether | HCID 86584777 | — |
| 生成物 | HCID 178485835 | HCID 178485835 | 101.9% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858651B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-28db14751ac646c88829af2b73dfd95f |
| 出典メモ | uspto-grants-2005_02 |