참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2-Nitrophenylacetonitrile | HCID 11888 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4,6-Dimethoxy-2-(methylsulfonyl)pyrimidine | HCID 838363 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(4,6-Dimethoxypyrimidine-2-yl)-2-(2-nitrophenyl)acetonitrile | HCID 18417990 | 79.2% |
반응 단계
50 g (0.31 M) of 2-(2-nitrophenyl)acetonitrile was dissolved in 500 ml of dimethylformamide. Thereto was added 24.7 g (0.62 M) of 60% sodium hydride. The mixture was stirred at room temperature for 2 hours. Then, 68 g (0.31 M) of 4,6-dimethoxy-2-methanesulfonylpyrimidine was added. The mixture was stirred at 80° C. for 1 hour to give rise to a reaction. The reaction mixture was poured into water, followed by neutralization with dilute hydrochloric acid. The mixture was subjected to extraction with ethyl acetate. The extract was washed with water, dried and subjected to vacuum distillation to remove the solvent. The residue was recrystallized from ethanol to obtain 73.3 g (yield: 79%) of 2-(4,6-dimethoxypyrimidine-2-yl)-2-(2-nitrophenyl)acetonitrile as a white powder (melting point: 88 to 89° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06458748B1 |
|---|
| 출처 데이터셋 | uspto-grants-2002_10 |
|---|
| ORD ID | ord-dd022a877f0f4698bbe28d430fdf74a2 |
|---|
| 출처 메모 | uspto-grants-2002_10 |
|---|