Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 2-Methyl-4-(6-phenylethynyl-pyridazin-3-ylamino)-butan-2-ol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 3-Chloro-6-(phenylethynyl)pyridazine | HCID 12680260 | — |
| 반응물 | 4-Amino-2-methylbutan-2-ol hydrochloride | HCID 42614560 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | 2-Methyl-4-(6-phenylethynyl-pyridazin-3-ylamino)-butan-2-ol | HCID 57516775 | 27% |
반응 단계
A solution of 3-chloro-6-(phenylethynyl)pyridazine (CAS 77778-15-5) (125 mg, 0.582 mmol) and 4-amino-2-methylbutan-2-ol hydrochloride (244 mg, 1.75 mmol, 3 equiv.) and triethylamine (206 mg, 284 ml, 2.04 mmol, 2 equiv.) in 1.25 ml of pyridine was heated 20 hours at 85° C. The solvent was removed in vaccuo. The residue was taken up in ethyl acetate/methanol, adsorbed onto 4 g of silica and purified on a 20 g flash chromatography column using a heptane/ethyl acetate 85:15 to 15:85 gradient to yield 44 mg (27% yield) of the title compound as a crystalline white solid, MS: m/e=282.2 (M+H+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08618296B2 |
| 출처 데이터셋 | uspto-grants-2013_12 |
| ORD ID | ord-dabcfa0603374051af56a5fe1e82fc33 |
| 출처 메모 | uspto-grants-2013_12 |