2-Aminopropanol → 2-[[6-[3-(Trifluoromethyl)phenyl]-3-pyridazinyl]amino]-1-propanol

HRID 1589460노트

반응식

HRID 1589460 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.[NH2:18][CH:19]([CH3:22])[CH2:20][OH:21]>O>[F:15][C:14]([F:17])([F:16])[C:10]1[CH:9]=[C:8]([C:5]2[N:4]=[N:3][C:2]([NH:18][CH:19]([CH3:22])[CH2:20][OH:21])=[CH:7][CH:6]=2)[CH:13]=[CH:12][CH:11]=1

참가 물질

4

반응물 2

HCID 51262-AminopropanolHCID 124495523-Chloro-6-[3-(trifluoromethyl)phenyl]pyridazine

생성물 1

HCID 135653562-[[6-[3-(Trifluoromethyl)phenyl]-3-pyridazinyl]amino]-1-propanol

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
130 °C

실험 절차

A mixture of 0.5 g of 3-chloro-6-[3-(trifluoromethyl)phenyl]pyridazine and 3 ml of 2-amino-1-propanol was heated at 130° C. for 24 hours, cooled and poured into water. The mixture was extracted with three 20 ml portions of dichloromethane. The combined extracts were washed with water, dried over magnesium sulfate and concentrated. The residual oil was dissolved in ethyl acetate and the solution passed through a short pad of silica gel. The filtrate was concentrated in vacuo and the residue was crystallized from dichloromethane-hexane to give 0.3 g of 2-[[6-[3-(trifluoromethyl)phenyl]-3-pyridazinyl]amino]-1-propanol as white crystals, mp 143°-144° C.

후처리

  1. temperaturecooled
  2. extractionThe mixture was extracted with three 20 ml portions of dichloromethane
  3. washThe combined extracts were washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated
  6. dissolutionThe residual oil was dissolved in ethyl acetate
  7. concentrationThe filtrate was concentrated in vacuo
  8. customthe residue was crystallized from dichloromethane-hexane

출처 및 근거

ORD 기록
ord-c67ee255125542b7bef92f122872e97e
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04569934

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