Ethyl Acetate → HCID 11827534、化合物

HRID 964351ノート

反応式

HRID 964351 の反応式
[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]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 24654Hydrazine hydrate (1:1)HCID 10929863HCID 10929863、化合物

生成物 1

HCID 11827534HCID 11827534、化合物収率 52.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d91dd6e1dfc648389c52877dcec5c714
出典データセット
uspto-grants-1998_06
特許番号
US05767296

反応ノート

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