Acetyl chloride → 5-Acetylamino-1-methyl-6-pyridazone

HRID 893182ノート

反応式

HRID 893182 の反応式
[C:1](Cl)(=[O:3])[CH3:2].[NH2:5][C:6]1[C:11](=[O:12])[N:10]([CH3:13])[N:9]=[CH:8][CH:7]=1>O1CCOCC1.N1C=CC=CC=1>[C:1]([NH:5][C:6]1[C:11](=[O:12])[N:10]([CH3:13])[N:9]=[CH:8][CH:7]=1)(=[O:3])[CH3:2]

参加物

5

反応物 2

HCID 6367Acetyl chlorideHCID 131036364-Amino-2-methyl-2,3-dihydropyridazin-3-one

生成物 1

HCID 146266165-Acetylamino-1-methyl-6-pyridazone収率 58%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
25 °C

実験手順

A solution of 2.7 ml of acetyl chloride in 20 ml of dioxane was added dropwise to a solution of 4.0 g (0.032 mol) of 5-amino-1-methyl-6-pyridazone in 100 ml of pyridine. After stirring for 12 hours at 25° C., the solvent was distilled off under reduced pressure, and the residue was taken up with methylene chloride, washed with sodium bicarbonate solution and dried. After the solvent had been stripped off under reduced pressure and the residue stirred with a small amount of diisopropyl ether, there was obtained 3.1 g (58.0%) of 5-acetylamino-1-methyl-6-pyridazone (active ingredient 1.001) of melting point 152°-153° C.

後処理

  1. distillationthe solvent was distilled off under reduced pressure
  2. washwashed with sodium bicarbonate solution
  3. customdried
  4. stirringthe residue stirred with a small amount of diisopropyl ether

出典と根拠

ORDレコード
ord-30ab794546f0402a8858c5bd6768c80b
出典データセット
uspto-grants-1992_06
特許番号
US05123952

反応ノート

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