Sodium Hydroxide → HCID 59436145, 화합물

HRID 1624622노트

반응식

HRID 1624622 반응식
[F:1][C:2]1([F:24])[O:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH:16]=[C:15]([O:17][CH3:18])[C:14](=[O:19])[C:13]([C:20]([O:22]C)=[O:21])=[N:12]3)[C:4]=2[O:3]1.[OH-].[Na+]>C1COCC1.CO>[F:24][C:2]1([F:1])[O:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([N:11]3[CH:16]=[C:15]([O:17][CH3:18])[C:14](=[O:19])[C:13]([C:20]([OH:22])=[O:21])=[N:12]3)[C:4]=2[O:3]1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 59436219Methyl 1-(2,2-difluoro-1,3-benzodioxol-4-yl)-1,4-dihydro-5-methoxy-4-oxo-3-pyridazinecarboxylate

생성물 1

HCID 59436145HCID 59436145, 화합물수율 97.1%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 1-(2,2-difluoro-1,3-benzodioxol-4-yl)-5-methoxy-4-oxo-1,4-dihydropyridazine-3-carboxylate (4.1 g, 12 mmol) in THF (100 mL) and MeOH (50 mL) was added 1 M NaOH aqueous solution (18 mL, 18 mmol), and the mixture was stirred at room temperature for 1 h. The mixture was concentrated under reduced pressure, and acidified with 1 M HCl aqueous solution. The mixture was diluted with AcOEt, washed with water and brine, dried over MgSO4, filtered and concentrated under reduced pressure to give the title compound (3.8 g, 97% yield) as a yellow amorphous solid: 1H NMR (300 MHz, CDCl3): δ ppm 4.06 (3H, s), 7.22-7.26 (1H, m), 7.34 (1H, t, J=8.3 Hz), 7.72 (1H, dd, J=8.3, 1.1 Hz), 8.29 (1H, s).

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additionThe mixture was diluted with AcOEt
  3. washwashed with water and brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-24b71382941a4331b4ca7dbc0b3c859b
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08778944B2

반응 노트

불러오는 중…