Hydrochloric Acid → HCID 23079541, 화합물

HRID 2102333노트

반응식

HRID 2102333 반응식
[CH2:1]([O:8][C:9]1[C:13]([C:14](O)=[O:15])=[C:12]([Br:17])[N:11]([CH:18]([CH3:20])[CH3:19])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.Cl>O1CCCC1>[CH2:1]([O:8][C:9]1[C:13]([CH2:14][OH:15])=[C:12]([Br:17])[N:11]([CH:18]([CH3:20])[CH3:19])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 230795363-Benzyloxy-5-bromo-1-isopropylpyrazole-4-carboxylic acid

생성물 1

HCID 23079541HCID 23079541, 화합물수율 68%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

3-Benzyloxy-5-bromo-1-isopropylpyrazole-4-carboxylic acid (4.6 g) was dissolved in tetrahydrofuran (30 mL), and borane-tetrahydrofuran complex, 1M tetrahydrofuran solution (21 mL) was delivered by drops into the stirred solution under ice cooling. The mixture was stirred at room temperature for 1 hour. The reaction mixture was cooled with ice bath, and water (50 mL) was delivered by drops into the mixture. Hydrochloric acid (1 mol/L, 20 mL) was delivered by drops into the mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by column chromatography on silica gel (eluent:ethyl acetate/hexane =1/5) to give the title compound (3.0 g).

후처리

  1. temperatureThe reaction mixture was cooled with ice bath
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe obtained residue was purified by column chromatography on silica gel (eluent:ethyl acetate/hexane =1/5)

출처 및 근거

ORD 기록
ord-d9f2ca69b33b4e7c848ee14771d8a9d2
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576063B2

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