Sodium Hydroxide → HCID 59436145、化合物

HRID 1805502ノート

反応式

HRID 1805502 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 59436145HCID 59436145、化合物収率 97.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-995aa21a70d24e028949da30d5d8e68a
出典データセット
uspto-grants-2013_01
特許番号
US08354411B2

反応ノート

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