참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | N,N-Dimethylaniline | HCID 949 | — |
| 반응물 | Diethyl Malonate | HCID 7761 | — |
| 반응물 | 1-Bromo-2-methylbutane, (+)- | HCID 5464167 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 반응물 | p-Heptyloxybenzamidine hydrochloride | HCID 12238503 | — |
| 반응물 | (S)-4,6-dichloro-2-(p-heptyloxyphenyl)-5-(2-methylbutyl)-pyrimidine | HCID 86743091 | — |
| 반응물 | HCID 178418361 | HCID 178418361 | — |
| 반응물 | HCID 178444047 | HCID 178444047 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | (S)-2-(p-Heptyloxyphenyl)-5-(2-methylbutyl)-pyrimidine | HCID 53993226 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05389290 |
|---|
| 출처 데이터셋 | uspto-grants-1995_02 |
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| ORD ID | ord-2b533768100c4e4dae509e76e64796f8 |
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| 출처 메모 | uspto-grants-1995_02 |
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