Calcium Carbonate → 2,1,3-Benzothiadiazol-5-ylmethanol
반응식
Br[CH2:2][C:3]1[CH:11]=[CH:10][C:6]2=[N:7][S:8][N:9]=[C:5]2[CH:4]=1.C(=O)([O-])[O-:13].[Ca+2]>O1CCOCC1.O>[OH:13][CH2:2][C:3]1[CH:11]=[CH:10][C:6]2=[N:7][S:8][N:9]=[C:5]2[CH:4]=1참가 물질
4
실험 절차
5-Bromomethylbenzo-2,1,3-thiadiazole (4.8 g) and calcium carbonate (10 g) were heated at reflux in 1:1 dioxane/water (120 mL) for 3 hours. The solvents were evaporated and the residue was partitioned between 2N hydrochloric acid and methylene 6 3 chloride. The organic layers were dried (magnesium sulfate), evaporated and chromatographed on silica gel eluting with 1:1 ethyl acetate/hexane to provide 2.66 g of the title compound.
후처리
- customThe solvents were evaporated
- customthe residue was partitioned between 2N hydrochloric acid and methylene 6 3 chloride
- dry with materialThe organic layers were dried (magnesium sulfate)
- customevaporated
- customchromatographed on silica gel eluting with 1:1 ethyl acetate/hexane
출처 및 근거
- ORD 기록
- ord-029bc9b646b04e428b99707522c2021c
- 출처 데이터셋
- uspto-grants-2003_07
- 특허 번호
- US06593335B1
반응 노트
불러오는 중…