Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
tert-Butanol → HCID 58874048, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | tert-Butanol | HCID 6386 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 반응물 | Thieno(2,3-b)pyridine-2-carboxylic acid | HCID 7162095 | — |
| 생성물 | HCID 58874048 | HCID 58874048 | — |
반응 단계
A solution of compound 147-C (0.36 g, 2.00 mmol), N,N-diisopropylethylamine (0.385 mL, 2.21 mmol) and diphenyl phosphoryl azide (0.536 mL, 2.41 mmol) in t-butanol (3.6 mL) was heated at reflux for 16 h. The solvent was evaporated in vacuo, the residue dissolved in dichloromethane, washed with 1 N NaOH, brine, dried with Na2SO4, filtered, and evaporated to afford a residue. Flash column chromatography (SiO2) eluting with dichloromethane afforded compound 147-D as a white solid (0.25 g, 50%). 1H-NMR (CDCl3): δ 1.55 (s, 9H), 6.60 (s, 1H), 7.20 (dd, 1H), 7.80 (d, 1H), 8.40 (d, 1H); MS: m/z 251.2 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08809327B2 |
| 출처 데이터셋 | uspto-grants-2014_08 |
| ORD ID | ord-7c82401eec0048d4b96021a2ac762465 |
| 출처 메모 | uspto-grants-2014_08 |