N-[4-(1-Ethyl-propyl)-6-methyl-pyridazin-3-yl]-2,2-dimethyl-propionamide → 6-Methyl-4-(pentan-3-YL)pyridazin-3-amine

HRID 226005노트

반응식

HRID 226005 반응식
[CH2:1]([CH:3]([C:6]1[CH:11]=[C:10]([CH3:12])[N:9]=[N:8][C:7]=1[NH:13]C(=O)C(C)(C)C)[CH2:4][CH3:5])[CH3:2]>Cl>[CH2:1]([CH:3]([C:6]1[CH:11]=[C:10]([CH3:12])[N:9]=[N:8][C:7]=1[NH2:13])[CH2:4][CH3:5])[CH3:2]

참가 물질

3

반응물 1

HCID 68842351N-[4-(1-Ethyl-propyl)-6-methyl-pyridazin-3-yl]-2,2-dimethyl-propionamide

생성물 1

HCID 534216106-Methyl-4-(pentan-3-YL)pyridazin-3-amine수율 82.2%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
95 °C

실험 절차

Dissolve 12.0 g (45 mmol) of N-[4-(1-ethyl-propyl)-6-methyl-pyridazin-3-yl]-2,2-dimethyl-propionamide in 60 ml of concentrated hydrochloric acid. Heat to 95° C. in a sealed flask for 2 h. Work up by pouring over ice and extracting with ethyl acetate three times. Discard the organic and adjust pH of aqueous to basic using 2N sodium hydroxide. Extract basic solution with ethyl acetate five times. Dry over magnesium sulfate, filter, and evaporate to obtain 6.68 g (37 mmol, 81.0%) of the title compound as brownish oil. 1H-NMR (DMSO-d6): δ 6.95 (s, 1H); 5.89 (s, br, 2H); 2.52-2.56 (m, 1H); 2.34 (s, 3H); 1.44-1.58 (m, 4H); 0.72 (t, J=7.04 Hz, 6H) ppm. MS/ES+=180 (100%, M+1).

후처리

  1. additionby pouring over ice
  2. extractionextracting with ethyl acetate three times
  3. extractionExtract basic solution with ethyl acetate five times
  4. dry with materialDry over magnesium sulfate
  5. filtrationfilter
  6. customevaporate

출처 및 근거

ORD 기록
ord-0a7e55e356254d93841da9005be59273
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07557103B2

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