반응식
C[O:2][C:3]([CH2:5][C:6]1[S:7][CH:8]=[CH:9][C:10]=1[C:11]([O:13]C)=[O:12])=[O:4].[OH-].[Na+]>CO.O>[C:3]([CH2:5][C:6]1[S:7][CH:8]=[CH:9][C:10]=1[C:11]([OH:13])=[O:12])([OH:4])=[O:2]참가 물질
5
실험 절차
13.0 g of the compound obtained in Example 1 was dissolved in 260 mL of methanol, and a solution obtained by dissolving 4.84 g of sodium hydroxide in 26 mL of water was added thereto. The resulting solution was refluxed for 4 hours, cooled to room temperature, concentrated under reduced pressure to remove methanol. The resulting aqueous solution was washed with 10 ml of diethyl ether and acidified to pH 2 to 3 using concentrated HCl. The solids thus solidified were filtered, washed with a small amount of cold water and dried at 40° C. to obtain 9.60 g (yield of 85%) of the title compound as a brown solid.
후처리
- customa solution obtained
- additionwas added
- temperatureThe resulting solution was refluxed for 4 hours
- concentrationconcentrated under reduced pressure
- customto remove methanol
- washThe resulting aqueous solution was washed with 10 ml of diethyl ether
- filtrationThe solids thus solidified were filtered
- washwashed with a small amount of cold water
- customdried at 40° C.
출처 및 근거
- ORD 기록
- ord-0f920847adf342cfad86735dfee72b9c
- 출처 데이터셋
- uspto-grants-2008_11
- 특허 번호
- US07449580B2
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