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

HRID 247365노트

반응식

HRID 247365 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매2회HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-00090178383f46be8306f997803f5ef6
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04707463

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