HCID 90030086, 화합물 → HCID 178494717, 화합물

HRID 1488183노트

반응식

HRID 1488183 반응식
C([N:8]1[CH:12]=[C:11]([CH3:13])[C:10]([CH2:14][O:15][CH3:16])=[N:9]1)C1C=CC=CC=1>CO>[CH3:16][O:15][CH2:14][C:10]1[C:11]([CH3:13])=[CH:12][NH:8][N:9]=1

참가 물질

3

반응물 1

HCID 90030086HCID 90030086, 화합물2회

생성물 1

HCID 178494717HCID 178494717, 화합물수율 122.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Into a 100-mL round-bottom flask, was placed a solution of 1-benzyl-3-(methoxymethyl)-4-methyl-1H-pyrazole (compound 268.3, 700 mg, 3.24 mmol) in methanol (10 mL). The system was purged with nitrogen, then Pd(OH)2/C (70 mg, 20 wt %) and aqueous HCl (2 M, 0.3 mL) were carefully added. The system was then charged with hydrogen (1 atm) and the resulting mixture was stirred for 2 days at room temperature. The system was purged with nitrogen, then the solids were removed by filtration and the filtrate was concentrated under reduced pressure. The pH of the residue was adjusted to 7 with aqueous sodium bicarbonate (sat.) and extracted with ethyl acetate (3×50 mL). The combined organic extracts were washed with brine (2×30 mL), dried (Na2SO4), filtered and concentrated under reduced pressure to obtain the title compound as a yellow oil (500 mg, crude).

후처리

  1. customInto a 100-mL round-bottom flask, was placed
  2. customThe system was purged with nitrogen
  3. additionPd(OH)2/C (70 mg, 20 wt %) and aqueous HCl (2 M, 0.3 mL) were carefully added
  4. additionThe system was then charged with hydrogen (1 atm)
  5. customThe system was purged with nitrogen
  6. customthe solids were removed by filtration
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. extractionextracted with ethyl acetate (3×50 mL)
  9. washThe combined organic extracts were washed with brine (2×30 mL)
  10. dry with materialdried (Na2SO4)
  11. filtrationfiltered
  12. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-87476995edc4491dbf8760a925b8877a
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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