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

HRID 990735노트

반응식

HRID 990735 반응식
[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]

참가 물질

4

반응물 3

HCID 107931,3-DichloroacetoneHCID 12957TrimethylacetamideHCID 14798Sodium Hydroxide

생성물 1

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

반응 조건

온도
135 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-120e4bb1a1d540faaba9e4e76c9da5bf
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06462049B1

반응 노트

불러오는 중…