Hydrochloric Acid → 1-(6-Methoxy-2-naphthalenyl)-1-propanone

HRID 1030849

反応式

HRID 1030849 の反応式
Br[C:2]1[C:11]([O:12][CH3:13])=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([C:14](=[O:17])[CH2:15][CH3:16])=[CH:7]2.[Cl-].[Al+3].[Cl-].[Cl-].Cl>C(Cl)Cl.C1(C)C=C(C)C=C(C)C=1>[CH3:13][O:12][C:11]1[CH:2]=[C:3]2[C:8](=[CH:9][CH:10]=1)[CH:7]=[C:6]([C:14](=[O:17])[CH2:15][CH3:16])[CH:5]=[CH:4]2

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14719981-(5-Bromo-6-methoxy-2-naphthyl)-1-propanoneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 759131-(6-Methoxy-2-naphthalenyl)-1-propanone

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 7947Mesitylene溶媒

反応条件

温度
-5 °C

実験手順

29.3 Grams of 5-bromo-6-methoxy-2-propionylnaphthalene are dissolved in 100 ml of anhydrous methylene chloride and in 20.8 ml of mesitylene. 20 Grams of anhydrous aluminum chloride are added portionwise to the reaction mixture cooled to -5° C. under strong stirring, while keeping the temperature below 20° C. The reaction mixture is kept for over 3 hours under stirring at room temperature, then it is slowly poured under strong stirring into a mixture made of 110 g of ice and of 35 ml of a 35% (w/v) aqueous solution of hydrochloric acid. The layers are separated after 15 minutes of stirring and the aqueous layer is discarded. The organic layer first is twice washed with 50 ml of a 6N aqueous solution of hydrochloric acid and then with 50 ml of water. The organic solution is then added with 50 ml of water and the pH is brought to 12 by means of a 30% (w/v) aqueous solution of sodium hydroxide.

後処理

  1. customthe temperature below 20° C
  2. customis kept for over 3 hours
  3. additionit is slowly poured
  4. stirringunder strong stirring into a mixture
  5. customThe layers are separated after 15 minutes
  6. stirringof stirring
  7. washThe organic layer first is twice washed with 50 ml of a 6N aqueous solution of hydrochloric acid
  8. additionThe organic solution is then added with 50 ml of water

出典と根拠

ORDレコード
ord-a3a1c3e82b284e659e7aa49220cf9398
出典データセット
uspto-grants-1992_04
特許番号
US05107013

関連ノート

読み込み中…