Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrogen Peroxide → 5-Chloro-6-((3,3-difluorocyclobutyl)methoxy)pyridin-3-OL
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrogen Peroxide | HCID 784 | — |
| 반응물 | Thiosulfite(2-) | HCID 9548651 | — |
| 반응물 | 3-Chloro-2-((3,3-difluorocyclobutyl)methoxy)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-YL)pyridine | HCID 58042483 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 5-Chloro-6-((3,3-difluorocyclobutyl)methoxy)pyridin-3-OL | HCID 58042389 | 81% |
반응 단계
3-Chloro-2-[(3,3-difluorocyclobutyl)methoxy]-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (Preparation 38, 4.5 g, 12.5 mmol) was suspended in methanol (30 mL). Hydrogen peroxide (1.6 mL, 21.3 mmol) was added and the mixture stirred at room temperature under nitrogen for 16 hours. An aqueous solution of thiosulfite (10%, 10 mL) was added and the mixture was extracted with EtOAc (2×200 mL). The combined organics were dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography (Biotage®, gradient of 0-50% EtOAc in heptane) to afford the title compound (2.53 g, 81%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09102621B2 |
| 출처 데이터셋 | uspto-grants-2015_08 |
| ORD ID | ord-760529be6cd646738e14bb8ab900c714 |
| 출처 메모 | uspto-grants-2015_08 |