Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Acetic Acid → HCID 59423435, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | 3-Methoxyaniline | HCID 10824 | — |
| 반응물 | Trimethylpyruvic acid | HCID 13150 | — |
| 반응물 | Sodium cyanoborohydride [MI] | HCID 20587905 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 59423435 | HCID 59423435 | 16% |
반응 단계
To a mixture of 3-methoxyaniline (100 mg, 0.812 mmol) and trimethylpyruvic acid (211 mg, 1.624 mmol) in methanol (3 mL) at rt was added acetic acid (0.930 mL, 16.24 mmol). The mixture was stirred for 30 min at rt then heated at 70° C. for 2 hrs. The mixture was cooled down to rt before adding sodium cyanotrihydroborate (1.624 mL, 1.624 mmol). The mixture was stirred overnight at rt. Water (10 mL) was added, and the mixture was extracted with ethyl acetate (3×10 mL). The organic layer was washed with sat. NaHCO3 and brine solution, and then dried over Na2SO4, filtered, and evaporated to dryness. The residue was purified by preparative HPLC to get a white solid (30.5 mg, 16%) as product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07888464B2 |
| 출처 데이터셋 | uspto-grants-2011_02 |
| ORD ID | ord-8b2252f6b0b145209cd06fcde3d55936 |
| 출처 메모 | uspto-grants-2011_02 |