Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonia acetate → 5,6-Dimethyl-2-phenylthieno[2,3-d]pyrimidin-4-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonia acetate | HCID 12432 | — |
| 반응물 | Benzene, (triethoxymethyl)- | HCID 74268 | — |
| 반응물 | 2-Amino-4,5-dimethyl-thiophene-3-carbonitrile | HCID 290236 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5,6-Dimethyl-2-phenylthieno[2,3-d]pyrimidin-4-amine | HCID 25224343 | 31% |
반응 단계
A mixture of 2-amino-4,5-dimethylthiophene-3-carbonitrile (152 mg, 1.0 mmol), ammonia acetate (308.3 mg, 4.0 mmol) and triethyl orthobenzoate (2.0 mL) in a sealed tube was put in a microwave at 200° C. for 20 min. After the reaction mixture was cooled to room temperature, it was diluted with EtOAc, washed with saturated NaHCO3 and H2O. The solvent was removed by vacuum and the residue was purified by preparative HPLC eluting with acetonitrile and water to give the title compound (80 mg, 31%). 1H NMR (400 MHz, CDCl3) δ2.45 (s, 3H), 2.48 (s, 3H), 5.34 (bs, 2H), 7.46-7.43 (m, 3H), 8.4-8.38 (m, 2H). MS 256 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08541421B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-31dbe6461de143a3a798065fdbe430cf |
| 출처 메모 | uspto-grants-2013_09 |