Ethanolamine → HCID 9883078, 화합물

HRID 1635494노트

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HRID 1635494 반응식
Cl[C:2]1[CH:7]=[C:6]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([CH3:19])[CH:14]=3)[N:11]=[C:10]([CH3:20])[CH:9]=2)[CH:5]=[CH:4][N:3]=1.[CH2:21]([CH2:23][NH2:24])[OH:22].C(OCC)(=O)C>O>[OH:22][CH2:21][CH2:23][NH:24][C:2]1[CH:7]=[C:6]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([CH3:19])[CH:14]=3)[N:11]=[C:10]([CH3:20])[CH:9]=2)[CH:5]=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 700EthanolamineHCID 8857Ethyl AcetateHCID 114829832-chloro-4-[1-(3-methylphenyl)-3-methyl-1H-pyrazol-5-yl]pyridine

생성물 1

HCID 9883078HCID 9883078, 화합물수율 80%

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

A mixture of 2-chloro-4-[1-(3-methylphenyl)-3-methyl-1H-pyrazol-5-yl]pyridine (Example 45; 0.5 g, 0.0018 mol) and ethanolamine (15 mL) was heated at 100° C. for 18 hours. The reaction mixture was cooled and treated with ethyl acetate and water. The organic layer was washed with brine, dried over magnesium sulfate and filtered. The filtrate was concentrated and the crude was purified by chromatography on silica gel (ethyl acetate) to give 0.44 g (80% yield) of product as a yellow oil: Anal. Calc'd. for C18H20N4O: C, 70.11; H, 6.54; N, 18.17. Found: C, 69.89; H, 6.65; N, 18.35.

후처리

  1. temperatureThe reaction mixture was cooled
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated
  6. customthe crude was purified by chromatography on silica gel (ethyl acetate)

출처 및 근거

ORD 기록
ord-33db547e1adf4f4fb31824a66de1d520
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06509361B1

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