1,3-Dichloroacetone → 2-tert-Butyl-4-(chloromethyl)-1,3-oxazole

HRID 1107689ノート

反応式

HRID 1107689 の反応式
[C:1]([NH2:7])(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].[Cl:8][CH2:9][C:10](=O)[CH2:11]Cl.[OH-].[Na+]>>[C:2]([C:1]1[O:6][CH:11]=[C:10]([CH2:9][Cl:8])[N:7]=1)([CH3:5])([CH3:4])[CH3:3]

参加物

4

反応物 3

HCID 107931,3-DichloroacetoneHCID 12957TrimethylacetamideHCID 14798Sodium Hydroxide

生成物 1

HCID 221695102-tert-Butyl-4-(chloromethyl)-1,3-oxazole収率 51.2%

反応条件

温度
135 °C

実験手順

25 g of pivalic acid amide and 25 g of 1,3-dichloro-2-propanone were mixed and heated on an oil bath at 135° C. for 2.5 hours. After having been cooled with ice, the mixture was made alkaline with an aqueous solution of sodium hydroxide added thereto. Then, the resulting product was extracted with ethyl acetate, washed with water, and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residual product was purified through column chromatography (silica gel; ethyl acetate n-hexane=1:8) to obtain 17.5 g of 2-tert-butyl-4-chloromethyloxazole.

後処理

  1. temperatureAfter having been cooled with ice
  2. additionadded
  3. extractionThen, the resulting product was extracted with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residual product was purified through column chromatography (silica gel; ethyl acetate n-hexane=1:8)

出典と根拠

ORDレコード
ord-b7e5e4bfc80b4bafa31284bfd40bd106
出典データセット
uspto-grants-2000_05
特許番号
US06063734

反応ノート

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