반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][OH:7].[H-].[Na+].[Cl:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13](Cl)[N:12]=1>O1CCCC1>[Cl:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([O:7][CH2:6][C:2]2[S:1][CH:5]=[CH:4][CH:3]=2)[N:12]=1참가 물질
5
실험 절차
To a solution containing 2-thiophenemethanol (1.5 g, 0.0135×1.0 mol) and sodium hydride (0.58 g, (ca.60% in mineral oil), 0.0135×1.1 mol) in tetrahydrofuran, 2,6-dichloropyridine (2.0 g, 0.0135 mol) was added and the resultant solution was refluxed for about 2 hours. The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate. The obtained organic layer was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and thereafter, concentrated and purified on a silica gel column to obtain the end product.
후처리
- additionwas added
- customThe reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
- washThe obtained organic layer was washed with aqueous saturated sodium chloride
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- custompurified on a silica gel column
- customto obtain the end product
출처 및 근거
- ORD 기록
- ord-03751012921c4d36a4cff78637b58504
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05624942
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