참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Sodium sulfate decahydrate | HCID 62649 | — |
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | Diisobutylaluminumhydride | HCID 21225700 | — |
| 반응물 | Ethyl 5-(difluoromethoxy)picolinate | HCID 68430338 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Pyridinemethanol, 5-(difluoromethoxy)- | HCID 68431756 | 87% |
반응 단계
A toluene solution (13.8 mL, 13.8 mmols) of 1N diisobutylaluminium hydride was added to a THF solution (40 mL) of 2-ethoxycarbonyl-5-difluoromethoxypyridine (1.0 g, 4.6 mols) and stirred at 0° C. for 40 minutes. Successively sodium borohydride (174 mg, 4.6 mmols) and methanol (2 mL) were added and stirred at 0° C. for 30 minutes. Sodium sulfate decahydrate was added to the reaction liquid and stirred overnight at room temperature. Filtering the insoluble matter with Celite, the solvent was concentrated under reduced pressure. The residue was purified on silica gel column chromatography (C-300, hexane:ethyl acetate=3:2-2:3) to provide the title compound (738 mg, 87%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07732456B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_06 |
|---|
| ORD ID | ord-2b2063a5771f49eaa882928ed87a2712 |
|---|
| 출처 메모 | uspto-grants-2010_06 |
|---|
