Benzene → 2-Propenoic acid, 3-phenyl-, 2-naphthalenyl ester

HRID 247365ノート

反応式

HRID 247365 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[OH:11].[OH-].[Na+].[C:14](Cl)(=[O:23])[CH:15]=[CH:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C1C=CC=CC=1>CC(C)=O.O>[C:14]([O:11][C:2]1[CH:3]=[CH:4][C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH:1]=1)(=[O:23])[CH:15]=[CH:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

7

反応物 4

HCID 241BenzeneHCID 86632-NaphtholHCID 14798Sodium HydroxideHCID 660233-Phenylprop-2-enoyl chloride

生成物 1

HCID 7852142-Propenoic acid, 3-phenyl-, 2-naphthalenyl ester収率 80.5%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒2 回HCID 962Water溶媒

実験手順

In 70 ml of acetone was dissolved 6.4 g of 2-naphthol. A 25% queous sodium hydroxide solution was added to the solution. A solution of 8.1 g of cinnamoyl chloride in 10 ml of acetone was dropwise added to the mixture over 4 minutes while stirring. After the stirring was continued for 7 minutes, benzene and water were added to the system to effect liquid separation. After the organic phase was washed with an aqueous hydrogen sodium carbonate solution, the system was dried over anhydrous potassium carbonate and the solvent was distilled off. The residue was treated with n-hexane and benzene to give crystals of the product. The product was recrystallized from a solvent mixture of n-hexane and benzene to give 9.8 g of the product.

後処理

  1. customliquid separation
  2. washAfter the organic phase was washed with an aqueous hydrogen sodium carbonate solution
  3. dry with materialthe system was dried over anhydrous potassium carbonate
  4. distillationthe solvent was distilled off
  5. additionThe residue was treated with n-hexane and benzene
  6. customto give crystals of the product
  7. customThe product was recrystallized from a solvent mixture of n-hexane and benzene

出典と根拠

ORDレコード
ord-00090178383f46be8306f997803f5ef6
出典データセット
uspto-grants-1987_11
特許番号
US04707463

反応ノート

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