Water → 3-[[5-(Trifluoromethyl)-2-pyridyl]oxy]-1-propanamine

HRID 49436노트

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HRID 49436 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][N:3]=1.[NH2:12][CH2:13][CH2:14][CH2:15][OH:16].O>C1COCC1.CC(C)([O-])C.[K+]>[F:9][C:8]([F:11])([F:10])[C:5]1[CH:6]=[CH:7][C:2]([O:16][CH2:15][CH2:14][CH2:13][NH2:12])=[N:3][CH:4]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 90863-Amino-1-propanolHCID 54637542-Fluoro-5-(trifluoromethyl)pyridine

생성물 1

HCID 221750853-[[5-(Trifluoromethyl)-2-pyridyl]oxy]-1-propanamine

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매3회HCID 23665647Potassium tert-butoxide용매

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온도
0 °C

실험 절차

2-Fluoro-5-trifluoromethylpyridine (1.831 g, 11 mmol) was dissolved in anhydrous THF (15 mL) with stirring under nitrogen and cooled to 0° C. in an ice bath. To this was added dropwise over 30 minutes a solution of 3-amino-1-propanol (0.76 mL, 10 mmol) in anhydrous THF (15 mL) and 1M potassium tert-butoxide in THF (10 mL, 10 mmol). The yellow solution was allowed to stir and slowly warm to room temperature overnight. The reaction mixture was poured into water (75 mL) and extracted with ether (2×50 mL). The organic phase was washed with brine (50 mL), dried (Na2SO4), filtered and evaporated under vacuum to a yellow liquid, which was nearly pure by NMR and MS, and was used as such without further purification.

후처리

  1. stirringto stir
  2. temperatureslowly warm to room temperature overnight
  3. extractionextracted with ether (2×50 mL)
  4. washThe organic phase was washed with brine (50 mL)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customevaporated under vacuum to a yellow liquid, which
  8. customsuch without further purification

출처 및 근거

ORD 기록
ord-d07a791be14640309bad24d49fc19a46
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706740B2

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