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Lithium Carbonate → Tert.-butyl 3-isopropyl-2-oxo-3-butenoate

HRID 972710
ノート
印刷プレビュー

反応式

HRID 972710 の反応式
[Br-].[Li+].Cl[C:4]1([O:17][C:12]1([CH:14]([CH3:16])[CH3:15])[CH3:13])[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6].C(=O)([O-])[O-].[Li+].[Li+]>O>[CH:14]([C:12](=[CH2:13])[C:4](=[O:17])[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6])([CH3:16])[CH3:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11125Lithium CarbonateHCID 82050Lithium BromideHCID 21443884Tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate

生成物 1

HCID 21405096Tert.-butyl 3-isopropyl-2-oxo-3-butenoate収率 85.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

118 g of anhydrous lithium bromide were added under an inert atmosphere to a mixture of 117.5 g of tert.butyl 2-chloro-2,3-epoxy-3-isopropyl-butanoate and 18.5 g of lithium carbonate in 1.15 liters of hexamethylphosphonotriamide cooled to 5° C. and after the temperature was returned to room temperature, the mixture was stirred under a nitrogen atmosphere for 48 hours. 500 ml of distilled water were added thereto and the mixture was poured into an ampoule containing a mixture of water-petroleum ether (9-1). The mixture was decanted and the aqueous phase was extracted with petroleum ether. The combined ether phases were washed with water, dried over magnesium sulfate and the petroleum ether was evaporated under reduced pressure to obtain 84.6 g of tert.-butyl 3-isopropyl-2-oxo-3-butenoate.

後処理

  1. customwas returned to room temperature
  2. additionthe mixture was poured into an ampoule
  3. additioncontaining
  4. customThe mixture was decanted
  5. extractionthe aqueous phase was extracted with petroleum ether
  6. washThe combined ether phases were washed with water
  7. dry with materialdried over magnesium sulfate
  8. customthe petroleum ether was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-d4c54c2751184d6b91375a4bec456f4e
出典データセット
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04053597

反応ノート

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