Nitrogen → 1-(3-Cyano-4-methoxyphenyl)-5-[4-(methylthio)phenyl]-2-pyrazoline-3-amine

HRID 429323

반응식

HRID 429323 반응식
Cl.[C:2]([C:4]1[CH:5]=[C:6]([NH:12][NH2:13])[CH:7]=[CH:8][C:9]=1[O:10][CH3:11])#[N:3].[CH3:14][S:15][C:16]1[CH:21]=[CH:20][C:19]([CH:22]=[CH:23][C:24]#[N:25])=[CH:18][CH:17]=1.C[O-].[Na+].N#N>CO.O.C(OCC)(=O)C>[C:2]([C:4]1[CH:5]=[C:6]([N:12]2[CH:22]([C:19]3[CH:20]=[CH:21][C:16]([S:15][CH3:14])=[CH:17][CH:18]=3)[CH2:23][C:24]([NH2:25])=[N:13]2)[CH:7]=[CH:8][C:9]=1[O:10][CH3:11])#[N:3]

참가 물질

8

반응물 4

HCID 947NitrogenHCID 42396803-[4-(Methylthio)phenyl]acrylonitrileHCID 10942334Sodium MethoxideHCID 18355391(3-Cyano-4-methoxyphenyl)hydrazine hydrochloride

생성물 1

HCID 183554041-(3-Cyano-4-methoxyphenyl)-5-[4-(methylthio)phenyl]-2-pyrazoline-3-amine수율 90.1%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
140 °C

실험 절차

A stirred mixture of (3-cyano-4-methoxyphenyl)hydrazine hydrochloride (3.7 g), 3-[4-(methylthio)phenyl]acrylonitrile (2.3 g) and sodium methoxide (0.9 g) in methanol 13 ml was gradually heated to 140° C. under atmospheric pressure and N2 atmosphere, and continued to heat for 8 hours at 140° C. Ethyl acetate and water were added to the reaction mixture. The organic layer was separated, washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure to give crude 1-(3-cyano-4-methoxyphenyl)-5-[4-(methylthio)-phenyl]-2-pyrazoline-3-amine (4.0 g).

후처리

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7b4b74057c9f41a9ae4432725fa8f793
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06316485B1

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