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

HRID 226005ノート

反応式

HRID 226005 の反応式
[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]

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
95 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0a7e55e356254d93841da9005be59273
出典データセット
uspto-grants-2009_07
特許番号
US07557103B2

反応ノート

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