Hydrochloric Acid → 6-chloro-3-hydroxy-2-(4-methylphenyl)-4H-1-benzopyran-4-one

HRID 260271

반응식

HRID 260271 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.[C:12]1([CH3:20])[CH:17]=[CH:16][C:15]([CH:18]=O)=[CH:14][CH:13]=1.[OH-:21].[Na+].OO.Cl>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:20]([C:12]3[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=3)=[C:9]([OH:21])[C:8](=[O:10])[C:6]=2[CH:7]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 77254-MethylbenzaldehydeHCID 14798Sodium Hydroxide2회HCID 740613-Chloro-6-hydroxyacetophenone

생성물 1

HCID 77466616-chloro-3-hydroxy-2-(4-methylphenyl)-4H-1-benzopyran-4-one

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A 8.5 g quantity of 5'-chloro-2'-hydroxyacetophenone and 6.0 g of p-tolualdehyde were dissolved in 105 ml of ethanol. Then 17 ml of an aqueous solution containing 10 g of sodium hydroxide was slowly added thereto dropwise and stirred at room temperature for 4 hours. Then 350 ml of ethanol and 17 ml of an aqueous solution containing 3.5 g of sodium hydroxide were added to the reaction mixture, and 8.3 ml of a 30% aqueous hydrogen peroxide solution was further added dropwise slowly and stirred at room temperature for 12 hours. A 10% aqueous HCl solution was added to adjust the reaction mixture to pH 3. The crystals precipitated were collected by filtration and washed serially with 10 ml of water, 5 ml of ethanol and 10 ml of diethyl ether, thus giving 6.0 g of 6-chloro-3-hydroxy-2-(4-methylphenyl)-4H-1-benzopyran-4-one as crystals.

후처리

  1. additionwas slowly added
  2. additionwas further added dropwise slowly
  3. stirringstirred at room temperature for 12 hours
  4. customThe crystals precipitated
  5. filtrationwere collected by filtration
  6. washwashed serially with 10 ml of water, 5 ml of ethanol and 10 ml of diethyl ether

출처 및 근거

ORD 기록
ord-1c3de887f27a413d90130333a19f58ab
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05527786

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