Periodate → 11beta-[4-[5-[(2-Pyridinylmethyl)sulphinyl]-pentyloxy]phenyl]estra-1,3,5(10)-triene-3,17beta-diol
반응식
I([O-])(=O)(=O)=O.[Na+].[N:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][S:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([C@H:27]2[CH2:44][C@@:42]3([CH3:43])[C@@H:38]([CH2:39][CH2:40][C@@H:41]3[OH:45])[C@H:37]3[C@H:28]2[C:29]2[CH:30]=[CH:31][C:32]([OH:46])=[CH:33][C:34]=2[CH2:35][CH2:36]3)=[CH:23][CH:22]=1.I([O-])(=O)(=O)=[O:48]>O.CO>[N:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH2:13][S:14]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][O:20][C:21]1[CH:22]=[CH:23][C:24]([C@H:27]2[CH2:44][C@@:42]3([CH3:43])[C@@H:38]([CH2:39][CH2:40][C@@H:41]3[OH:45])[C@H:37]3[C@H:28]2[C:29]2[CH:30]=[CH:31][C:32]([OH:46])=[CH:33][C:34]=2[CH2:35][CH2:36]3)=[CH:25][CH:26]=1)=[O:48]참가 물질
6
반응물 3
생성물 1
시약·촉매·용매 2
실험 절차
3.7 cm3 of a 0.1M solution of sodium metaperiodate in water is added to a solution of 172 mg of the product obtained in Example 4 in 12 cm3 of methanol. The reaction medium is agitated for 1 hour 30 minutes and 3.4 cm3 of methanol and 0.6 cm3 of the metaperiodate solution are added, after 3 hours 30 minutes of agitation the reaction medium is poured into water, extracted with ethyl acetate, washed with salt water and evaporated to dryness under reduced pressure. 176 mg of residue is obtained which is chromatographed on silica twice (eluant methylene chloride-methanol (92.5-7.5)). 107 mg of desired product is collected.
후처리
- extractionextracted with ethyl acetate
- washwashed with salt water
- customevaporated to dryness under reduced pressure
출처 및 근거
- ORD 기록
- ord-b1e3380efb0b42be95c5068b836a0743
- 출처 데이터셋
- uspto-grants-2003_07
- 특허 번호
- US06596885B2
반응 노트
불러오는 중…