Water → 4-chloro-2-(4-chlorophenyl)-5-(2,4-dichlorobenzyloxy)-3(2H)-pyridazinone

HRID 1165435

반응식

HRID 1165435 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]=[C:24]([Cl:26])[CH:23]=[CH:22][C:19]=1[CH2:20]Cl.C(N(CC)CC)C.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][CH2:20][C:19]1[CH:22]=[CH:23][C:24]([Cl:26])=[CH:25][C:18]=1[Cl:17]

참가 물질

6

반응물 4

HCID 962WaterHCID 72122,4-Dichlorobenzyl chlorideHCID 8471TriethylamineHCID 546974414-Chloro-2-(4-chlorophenyl)-5-hydroxypyridazin-3(2H)-one

생성물 1

HCID 140722464-chloro-2-(4-chlorophenyl)-5-(2,4-dichlorobenzyloxy)-3(2H)-pyridazinone수율 70%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 50 ml of N,N-dimethylformamide were dissolved 1.5 g (5.9 m mol) of 4-chloro-2-(4-chlorophenyl)-5-hydroxy-3(2H)-pyridazinone and 1.3 g (6.6 m mol) of 2,4-dichlorobenzyl chloride, and thereto was added 0.7 g of triethylamine. The reaction mixture was heated under stirring on an oil bath at 100° to 120° C. for 7 hours. After allowing to cool, the reaction mixture was poured into 200 ml of water and the precipitated solid was taken out by filtration, washed with water, dried and then recrystallized from benzene to give 1.7 g of the intended compound.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto cool
  3. filtrationthe precipitated solid was taken out by filtration
  4. washwashed with water
  5. customdried
  6. customrecrystallized from benzene

출처 및 근거

ORD 기록
ord-11726e65d5724958bfad5df91ff0ff55
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04910201

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