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

HRID 1165435

反応式

HRID 1165435 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-11726e65d5724958bfad5df91ff0ff55
出典データセット
uspto-grants-1990_03
特許番号
US04910201

関連ノート

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