HCID 67809616, 화합물 → HCID 19389468, 화합물
반응식
[Si:1]([O:8][CH2:9][CH:10]1[O:15][C:14](=[O:16])[CH:13]=[C:12]([OH:17])[CH2:11]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]>C(O)C>[Si:1]([O:8][CH2:9][CH:10]1[O:15][C:14](=[O:16])[CH2:13][CH:12]([OH:17])[CH2:11]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]참가 물질
3
실험 절차
6-t-Butyldimethylsilyloxymethyl-5,6-dihydro-4-hydroxy pyran-2-one (26.3 parts) was dissolved in ethanol (500 parts) and heated to 45° C.-55° C. Raney nickel (6.6 parts) was washed caustic free with water and then water free with ethanol and added to the pyran-2-one solution under a blanket of nitrogen. Hydrogen was passed through the rapidly stirred mixture until the reaction was complete, as judged by GC analysis. The catalyst was filtered off and the solvent removed at 40° C./20 mm to leave 6-t-butyldimethylsilyloxymethyl-4-hydroxytetrahydro pyran-2-one (25.7 parts, 96%, cis/trans ratio 82/18) as a greenish oil which solidified on standing.
후처리
- temperatureheated to 45° C.-55° C
- washRaney nickel (6.6 parts) was washed caustic free with water
- additionwater free with ethanol and added to the pyran-2-one solution under a blanket of nitrogen
- filtrationThe catalyst was filtered off
- customthe solvent removed at 40° C./20 mm
출처 및 근거
- ORD 기록
- ord-10fca33d8a424f7f8797511275ff703f
- 출처 데이터셋
- uspto-grants-1995_08
- 특허 번호
- US05443970
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