Water → 3(2H)-Pyridazinone, 4-chloro-2-(4-chlorophenyl)-5-((4-chlorophenyl)methoxy)-

HRID 1165426

반응식

HRID 1165426 반응식
[Cl:1][C:2]1[C:3](=[O:16])[N:4]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)[N:5]=[CH:6][C:7]=1[OH:8].[Cl:17][C:18]1[CH:25]=[CH:24][C:21]([CH2:22]Cl)=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:1][C:2]1[C:3](=[O:16])[N:4]([C:9]2[CH:10]=[CH:11][C:12]([Cl:15])=[CH:13][CH:14]=2)[N:5]=[CH:6][C:7]=1[O:8][CH2:22][C:21]1[CH:24]=[CH:25][C:18]([Cl:17])=[CH:19][CH:20]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 77231-Chloro-4-(chloromethyl)benzeneHCID 11430Potassium CarbonateHCID 546974414-Chloro-2-(4-chlorophenyl)-5-hydroxypyridazin-3(2H)-one

생성물 1

HCID 30652303(2H)-Pyridazinone, 4-chloro-2-(4-chlorophenyl)-5-((4-chlorophenyl)methoxy)-수율 59.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 70 ml of N,N-dimethylformamide was dissolved 7.1 g (0.028 mol) of 4-chloro-2-(4-chlorophenyl)-5-hydroxy-3(2H)-pyridazinone, and thereto were added 4.5 g of p-chlorobenzyl chloride and 5.4 g of anhydrous potassium carbonate. The resulting reaction mixture was heated under stirring on an oil bath at 120° to 130° C. for 2 hours. After allowing to cool, the reaction mixture was poured into 500 ml of water. The solid thus precipitated was taken out by filtration, washed with water, dried and then recrystallized from an ethyl acetate-benzene mixture to give 6.3 g of the intended compound.

후처리

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureto cool
  4. customThe solid thus precipitated
  5. filtrationwas taken out by filtration
  6. washwashed with water
  7. customdried
  8. customrecrystallized from an ethyl acetate-benzene mixture

출처 및 근거

ORD 기록
ord-d6219f38236f43bf825b5b80f8353636
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04910201

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