참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-Chloro-2-(methylthio)pyrimidine-5-carboxylic acid ethyl ester | HCID 80008 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | Ethyl 4-(methylamino)-2-(methylsulfanyl)pyrimidine-5-carboxylate | HCID 295697 | 81% |
반응 단계
To a solution of 4-chloro-2-methylsulfanyl-5-pyrimidinecarboxylate ethyl ester (18.66 g, 80.4 mmol) in 260 mL of tetrahydrofuran was added triethylamine (34 mL, 244 mmol), followed by 30 mL of a 40% aqueous solution of methylamine. The solution was stirred for 30 minutes at 25° C. then concentrated in vacuo and partitioned between chloroform and saturated aqueous sodium bicarbonate. The organic layer was washed with brine, dried over MgSO4, filtered, and concentrated to provide a white solid. The solid was suspended in hexane and filtered to provide 14.70 g (81%) of 4-methylamino-2-methylsulfanyl-5-pyrimidinecarboxylate ethyl ester, mp 91°-93° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05620981 |
|---|
| 출처 데이터셋 | uspto-grants-1997_04 |
|---|
| ORD ID | ord-b68eeee6024948cfad0d45fea499ee21 |
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| 출처 메모 | uspto-grants-1997_04 |
|---|
