Water → (Dimethyl-1,3-thiazol-5-yl)methanol
반응식
[CH3:1][C:2]1[S:3][C:4]([C:8](OCC)=[O:9])=[C:5]([CH3:7])[N:6]=1.[H-].[Li+].[Al+3].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[CH3:1][C:2]1[S:3][C:4]([CH2:8][OH:9])=[C:5]([CH3:7])[N:6]=1참가 물질
6
실험 절차
A solution of ethyl 2,4-dimethyl-1,3-thiazole-5-carboxylate (5.0 g) in THF (50 ml) was added dropwise to a solution of aluminum lithium hydride (1.1 g) in THF (150 ml) under ice-cooling. After stirred at room temperature for 4 hours, water (1.1 ml), 15% sodium hydroxide solution (1.1 ml) and water (3.3 ml) were added thereto, and the mixture was stirred for 10 minutes. The mixture was filtered with Celite, and washed with methanol. The solvent was removed under reduced pressure, and the resulting residue was purified with silica gel column chromatography (hexane/ethyl acetate=1/2) to give (2,4-dimethyl-1,3-thiazol-5-yl)methanol (2.0 g).
후처리
- temperaturecooling
- stirringthe mixture was stirred for 10 minutes
- filtrationThe mixture was filtered with Celite
- washwashed with methanol
- customThe solvent was removed under reduced pressure
- customthe resulting residue was purified with silica gel column chromatography (hexane/ethyl acetate=1/2)
출처 및 근거
- ORD 기록
- ord-be281974150d4bd69f65e71a28bc3d4f
- 출처 데이터셋
- uspto-grants-2005_08
- 특허 번호
- US06936602B1
반응 노트
불러오는 중…