関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N-Dimethylaniline | HCID 949 | — |
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | 1-Bromo-2-methylbutane, (+)- | HCID 5464167 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | p-Heptyloxybenzamidine hydrochloride | HCID 12238503 | — |
| 反応物 | (S)-4,6-dichloro-2-(p-heptyloxyphenyl)-5-(2-methylbutyl)-pyrimidine | HCID 86743091 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 反応物 | HCID 178444047 | HCID 178444047 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | (S)-2-(p-Heptyloxyphenyl)-5-(2-methylbutyl)-pyrimidine | HCID 53993226 | — |
反応手順
A mixture of 40 g of (S)-4,6-dichloro-2-(p-heptyloxyphenyl)-5-(2-methylbutyl)-pyrimidine [obtainable by reacting (S)-2-methylbutyl bromide with diethyl malonate in the presence of sodium methanolate, followed by condensation of the resultant diethyl (S)-2-methylbutyl malonate with p-heptyloxybenzamidine hydrochloride, and reacting the resultant (S)-4,6-dihydroxy-2-(p-heptyloxyphenyl)-5-(2-methylbutyl)-pyrimidine with phosphoroxy trichloride and dimethylaniline], 400 ml of methanol, 40 ml of triethylamine and 20 g of Pd-C (5%) is hydrogenated at room temperature under normal pressure until the theoretical amount of hydrogen has been taken up. After filtering off the catalyst and distilling off the solvent, the residue is recrystallized from ethanol. (S)-2-(p-Heptyloxyphenyl)-5-(2-methylbutyl)-pyrimidine is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05389290 |
|---|
| 出典データセット | uspto-grants-1995_02 |
|---|
| ORD ID | ord-2b533768100c4e4dae509e76e64796f8 |
|---|
| 出典メモ | uspto-grants-1995_02 |
|---|
