Ethyl Acetate → HCID 11827534, 화합물

HRID 964351노트

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HRID 964351 반응식
[CH3:1][C:2]1[C@@H:19]([OH:20])[CH2:18][C@:14]2([OH:21])[C:15]([CH3:17])([CH3:16])[C:3]=1[C@@H:4]([O:38]C(C)=O)[C:5]([C@@:7]1([CH3:37])[C@H:12]([C@@H:13]2[O:22][C:23]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:24])[C@:11]2([O:33][C:34]([CH3:36])=[O:35])[CH2:31][O:32][C@@H:10]2[CH2:9][CH2:8]1)=[O:6].O.NN.C(OCC)(=O)C>C(O)C>[CH3:1][C:2]1[C@@H:19]([OH:20])[CH2:18][C@:14]2([OH:21])[C:15]([CH3:16])([CH3:17])[C:3]=1[C@@H:4]([OH:38])[C:5]([C@@:7]1([CH3:37])[C@H:12]([C@@H:13]2[O:22][C:23]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[O:24])[C@:11]2([O:33][C:34]([CH3:36])=[O:35])[CH2:31][O:32][C@@H:10]2[CH2:9][CH2:8]1)=[O:6]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 24654Hydrazine hydrate (1:1)HCID 10929863HCID 10929863, 화합물

생성물 1

HCID 11827534HCID 11827534, 화합물수율 52.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

6.85 g of 7-deoxybaccatin III was dissolved in 250 ml of 95% ethanol, and 25 ml of hydrazine monohydrate was added thereto, followed by stirring at room temperature for 7 hours. Ethyl acetate was added to the reaction solution, the resulting mixture was washed successively with water and a saturated aqueous sodium chloride solution, and the organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel thin layer chromatography (a developing solvent; hexane:ethyl acetate=3:2 (v/v)) to yield 3.34 g of the titled compound as colorless crystals.

후처리

  1. washthe resulting mixture was washed successively with water
  2. dry with materiala saturated aqueous sodium chloride solution, and the organic layer was dried over anhydrous sodium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe resulting residue was purified by silica gel thin layer chromatography (a developing solvent

출처 및 근거

ORD 기록
ord-d91dd6e1dfc648389c52877dcec5c714
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05767296

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