Acetone → 3-(2,4-dichlorophenyl)-6-methyl-2(1H)-pyridone

HRID 1003986

반응식

HRID 1003986 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9](=[CH:12]O)[C:10]#[N:11].[CH3:14][C:15]([CH3:17])=O.[OH-:18].[K+]>C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:10](=[O:18])[NH:11][C:15]([CH3:17])=[CH:14][CH:12]=1

참가 물질

5

반응물 3

HCID 180AcetoneHCID 14797Potassium HydroxideHCID 14830692-(2,4-Dichlorophenyl)-3-hydroxyprop-2-enenitrile

생성물 1

HCID 184083253-(2,4-dichlorophenyl)-6-methyl-2(1H)-pyridone수율 45%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
130 °C

실험 절차

α-(2,4-dichlorophenyl)-α-hydroxymethylene acetonitrile and 8.8 g of acetone were thoroughly mixed with 110 g of polyphosphoric acid, and the mixture was heated to about 130° C. At this temperature, an exothermic reaction started. The temperature was maintained from 130 to 140° C. for 30 minutes, while heating as the case required. The cooled mixture was poured into ice water, and this suspension was stirred for 18 hours. This crude product was stirred with ethyl acetate and an excess amount of a dilute aqueous potassium hydroxide solution to make it alkaline. The formed precipitate was collected by filtration and washed sequentially with water, ethyl acetate and diethyl ether to obtain 8.0 g (yield: 45%) of the desired product. Melting point: 266-268° C.

후처리

  1. customAt this temperature, an exothermic reaction
  2. temperatureThe temperature was maintained from 130 to 140° C. for 30 minutes
  3. temperaturewhile heating as the case
  4. filtrationThe formed precipitate was collected by filtration
  5. washwashed sequentially with water, ethyl acetate and diethyl ether

출처 및 근거

ORD 기록
ord-74f41da586314de9afc8b109a0516cec
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06048823

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