Benzaldehyde → Ccris 2231

HRID 2101226

反応式

HRID 2101226 の反応式
[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

参加物

5

反応物 3

HCID 240BenzaldehydeHCID 74764'-MethoxyacetophenoneHCID 14798Sodium Hydroxide

生成物 1

HCID 92853Ccris 2231

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
-10 °C

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-cd240694c7424362b56b277d201e586f
出典データセット
uspto-grants-2009_08
特許番号
US07572831B2

関連ノート

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