Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 4-(2-Morpholin-4-ylethoxy)benzeneboronic acid, pinacol ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 2-Morpholinoethanol | HCID 61163 | — |
| 반응물 | 4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)phenol | HCID 2734624 | — |
| 반응물 | Diisopropyl azodicarboxylate | HCID 5363146 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-(2-Morpholin-4-ylethoxy)benzeneboronic acid, pinacol ester | HCID 4625910 | 74% |
반응 단계
To a stirring solution of 4-(4,4,5,5-tetramethyl[1,3,2]dioxaborolan-2-yl)-phenol (2.55 g, 11.58 mmol), 2-morpholin-4-ylethanol (1.60 mL, 1.73 g, 13.2 mmol) and triphenyl phosphine (3.64 g, 13.9 mmol) in methylene chloride (60 mL) at 0° C. was added dropwise DIAD (2.82 g, 13.9 mmol). The reaction was allowed to warm to room temperature and stir overnight. After 18 hours, additional portions of triphenyl phosphine (1.51 g, 5.8 mmol), 2-morpholin-4-ylethanol (0.70 mL, 5.8 mmol), and DIAD (1.17 g, 5.8 mmol) were added. After stirring an additional 2 hours at room temperature the reaction was concentrated and the residue purified by flash chromatography (5% to 25% EtOAc in CHCl3) to provide the product as a white solid (2.855 g, 74%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08980890B2 |
| 출처 데이터셋 | uspto-grants-2015_03 |
| ORD ID | ord-e9dfdb1ce0c24ee588da2c8ed0b99059 |
| 출처 메모 | uspto-grants-2015_03 |