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

HRID 1589461

반응식

HRID 1589461 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 221292-Amino-1-butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2d8f46115af044c68d9b8ec912423530
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04569934

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