Water → 2-Ethyl-6-[3-(trifluoromethyl)phenyl]imidazo[1,2-b]pyridazine

HRID 1589461ノート

反応式

HRID 1589461 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)=[CH:6][CH:7]=1.O>NC(CC)CO>[CH2:6]([C:5]1[N:4]=[C:2]2[CH:7]=[CH:6][C:5]([C:8]3[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=3)=[N:4][N:3]2[CH:8]=1)[CH3:7]

参加物

4

反応物 2

HCID 962WaterHCID 124495523-Chloro-6-[3-(trifluoromethyl)phenyl]pyridazine

生成物 1

HCID 202465672-Ethyl-6-[3-(trifluoromethyl)phenyl]imidazo[1,2-b]pyridazine

試薬・触媒・溶媒 1

HCID 221292-Amino-1-butanol溶媒

実験手順

A 2.58 g sample of 3-chloro-6-[3-(trifluoromethyl)phenyl]pyridazine in 3.56 g of 2-amino-1-butanol was heated at 120° C. (internal temperature) for 18 hours, cooled and poured into cold water. The mixture was extracted with dichloromethane and the extracts washed with water, dried over anhydrous sodium sulfate and concentrated. The residue in ethyl acetate was chromatographed on silica gel with ethyl acetate to give 2.2 g of yellow oil. Crystallization from dichloromethane-hexane gave 2-{[6-[3-(trifluoromethyl)phenyl]-3-pyridazinyl]amino}-1-butanol as crystals, mp 84°-87° C.

後処理

  1. temperaturecooled
  2. extractionThe mixture was extracted with dichloromethane
  3. washthe extracts washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe residue in ethyl acetate was chromatographed on silica gel with ethyl acetate

出典と根拠

ORDレコード
ord-2d8f46115af044c68d9b8ec912423530
出典データセット
uspto-grants-1986_02
特許番号
US04569934

反応ノート

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