Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonia → 6-Chloro-2-methylsulfanylpyrimidine-4-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Methyl 6-chloro-2-(methylsulfanyl)pyrimidine-4-carboxylate | HCID 238726 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 6-Chloro-2-methylsulfanylpyrimidine-4-carboxamide | HCID 239276 | 103.4% |
반응 단계
A 500 mL flask was charged with the 6-chloro-2-methylsulfanyl-pyrimidine-4-carboxylic acid methyl ester (4.37 g, 20 mmol), and chloroform (30 mL). Ammonia (57 mL, 7 M in methanol, 0.4 mol, 20 eq.) was added with stirring. HPLC analysis after 20 minutes indicated no starting methyl ester remained. The mixture was sparged with nitrogen for 30 min, then concentrated in vacuo, and dried under high vacuum to afford the 6-chloro-2-methylsulfanyl-pyrimidine-4-carboxylic acid amide (4.21 g, quant.) in sufficient purity for use in the next step. 1H NMR (500 MHz, CDCl3) □ 7.76 (s, 1H), 7.60 (br s, 1H), 5.97 (br s, 1H), 2.61 (s, 3H); ESI-MS m/z 204.1 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822451B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-fbe7dfd91d8d45e19fc12674d442f8ad |
| 출처 메모 | uspto-grants-2014_09 |