Hydrochloric Acid → HCID 97793、化合物

HRID 1380809ノート

反応式

HRID 1380809 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]=O)=[CH:7][CH:8]=1.[CH3:11][C:12]([C:14]1[CH:15]=[CH:16][C:17]([OH:20])=[CH:18][CH:19]=1)=[O:13].[OH-].[Na+].Cl>O.C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH:9]=[CH:11][C:12]([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)=[O:13])=[CH:7][CH:8]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 74694'-HydroxyacetophenoneHCID 14798Sodium HydroxideHCID 312444-Methoxybenzaldehyde

生成物 1

HCID 97793HCID 97793、化合物収率 80.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

Into an ethanol solution (5 liters) comprising 500 g (3.67 moles) of anisaldehyde and 500 g (3.67 moles) of 4-hydroxyacetophenone was dropped an aqueous solution (600 ml) of 250 g of sodium hydroxide in about 80 minutes in a stream of nitrogen. Thereafter, the mixture was heated to 50° C. and agitated for 24 hours. The reaction mixture was cooled down to room temperature, to which were added 2 liters of 12% hydrochloric acid and then 4 liters of water, whereupon crystals settled. The crystals were collected by filtration and quickly washed with ethanol, followed by drying under reduced pressure to obtain 750 g of the intended compound (2.95 moles, yield 80%). The compound was recrystallized from ethanol to obtain light yellow prismatic purified crystals. The melting point and various spectral data of the compound coincided with those of a reference compound.

後処理

  1. temperatureThe reaction mixture was cooled down to room temperature, to which
  2. filtrationThe crystals were collected by filtration
  3. washquickly washed with ethanol
  4. customby drying under reduced pressure

出典と根拠

ORDレコード
ord-484a2375440d4a7399be83a465002d68
出典データセット
uspto-grants-1986_04
特許番号
US04584190

反応ノート

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