Benzaldehyde → Ccris 2231

HRID 2101226

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HRID 2101226 반응식
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][CH:5]=1)=[O:3].[OH-].[Na+].[CH:14](=O)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>CO>[CH3:11][O:10][C:7]1[CH:8]=[CH:9][C:4]([C:2](=[O:3])[CH:1]=[CH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 74764'-MethoxyacetophenoneHCID 14798Sodium Hydroxide

생성물 1

HCID 92853Ccris 2231

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
-10 °C

실험 절차

4-Methoxyacetophenone (1.4 g) and sodium hydroxide (0.2 g) were suspended in 15 Ml of methanol pre-chilled at −10° C. The solution was kept for 1 hr under 0° C. with stirring. Benzaldehyde (1 g) was added thereto, and refluxed for 10 hr at room temperature with stirring. After neutralization with 5% hydrochloric acid solution, the product was extracted with 100 Ml of ethylacetate. The extracted organic phase was dried with anhydrous magnesium sulfate, and evaporated under vacuum. The resulting 1.3 g of white powder was purified through silica gel column chromatography (5×3 cm, Merk), which is eluted with n-hexane:ethylacetate (v/v, 1:7). The purified compound was identified as follows:

후처리

  1. temperaturerefluxed for 10 hr at room temperature
  2. stirringwith stirring
  3. extractionAfter neutralization with 5% hydrochloric acid solution, the product was extracted with 100 Ml of ethylacetate
  4. dry with materialThe extracted organic phase was dried with anhydrous magnesium sulfate
  5. customevaporated under vacuum
  6. customThe resulting 1.3 g of white powder was purified through silica gel column chromatography (5×3 cm, Merk), which
  7. washis eluted with n-hexane

출처 및 근거

ORD 기록
ord-cd240694c7424362b56b277d201e586f
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07572831B2

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