Acetone → Benzo[1,3]dioxole-2,2-dicarboxylic acid diethyl ester

HRID 346270

反応式

HRID 346270 の反応式
[O:1]1[CH2:5][CH2:4]NC1=O.Br[CH:8]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10].[C:19](=[O:22])([O-])[O-].[K+].[K+].[CH3:25][C:26]([CH3:28])=O>>[O:22]1[C:19]2[CH:25]=[CH:26][CH:28]=[CH:4][C:5]=2[O:1][C:8]1([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

5

反応物 4

HCID 180AcetoneHCID 11430Potassium CarbonateHCID 69637Diethyl bromomalonateHCID 739492-Oxazolidinone

生成物 1

HCID 12969876Benzo[1,3]dioxole-2,2-dicarboxylic acid diethyl ester

実験手順

A mixture of 240 mg of the above oxazolidinone, 234 mg of diethyl bromomalonate, 450 mg of anhydrous potassium carbonate and 10 ml of acetone is stirred overnight, filtered, washed with acetone and evaporated to a brown oil. The oil is purified by flash chromatography, eluting with 5 percent acetone in toluene. The pure fractions are combined and evaporated giving 237 mg of (R,R)-5-(3-chlorophenyl)-2-oxo-3-oxazolidinyl)propyl)-1,3-benzodioxole-2,2-dicarboxylic acid, diethyl ester as a colorless oil.

後処理

  1. filtrationfiltered
  2. washwashed with acetone
  3. customevaporated to a brown oil
  4. customThe oil is purified by flash chromatography
  5. washeluting with 5 percent acetone in toluene
  6. customevaporated

出典と根拠

ORDレコード
ord-a24137a92f3c46a4af9ddc3777156183
出典データセット
uspto-grants-1991_10
特許番号
US05061727

関連ノート

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