Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 3-Amino-4-methylthiophene-2-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Methyl 3-amino-4-methylthiophene-2-carboxylate | HCID 123584 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-Amino-4-methylthiophene-2-carboxylic acid | HCID 14989678 | 84.5% |
반응 단계
To a solution of methyl 3-amino-4-methyl-2-thiophene carboxylate (5 g, 29 mmol) and sodium hydroxide (3.5 g, 88 mmol) in a mixed solution (methanol:H2O/30 ml:120 ml) was heated at 50° C. for over night. The solution was cooled to room temperature and extracted with methylene chloride. The aqueous phase was acidified with 6N HCl until pH equal to 5. The aqueous phase was extracted again with ethyl acetate, and solvent phase washed with brine and dried over by sodium sulfate. After filtered and dried over the solvent, evaporated solvent to give 3.85 g of 3-amino-4-methyl-thiophene-2-carboxylic acid as a white solid in 84% yield: 1H NMR (300 MHz, CDCl3) δ 7.05 (d, 1H), 3.12 (br, 2H), 2.16 (s, 3H); MS (m/e): 157.9 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08552186B2 |
| 출처 데이터셋 | uspto-grants-2013_10 |
| ORD ID | ord-d956a7d8d528484f8e7fb82ff4d46ae8 |
| 출처 메모 | uspto-grants-2013_10 |