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

HRID 893182노트

반응식

HRID 893182 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 146266165-Acetylamino-1-methyl-6-pyridazone수율 58%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 312751,4-Dioxane용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-30ab794546f0402a8858c5bd6768c80b
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05123952

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