Sodium Hydroxide → 3-(2-methyl-2H-pyrazol-3-yl)-4-(2-methyl-2-nitropropoxy)aniline

HRID 521641ノート

反応式

HRID 521641 の反応式
[OH-].[Na+].[CH3:3][N:4]1[C:8]([C:9]2[CH:10]=[C:11]([NH:23]C(=O)C)[CH:12]=[CH:13][C:14]=2[O:15][CH2:16][C:17]([CH3:22])([N+:19]([O-:21])=[O:20])[CH3:18])=[CH:7][CH:6]=[N:5]1>O.CO>[CH3:3][N:4]1[C:8]([C:9]2[CH:10]=[C:11]([CH:12]=[CH:13][C:14]=2[O:15][CH2:16][C:17]([CH3:22])([N+:19]([O-:21])=[O:20])[CH3:18])[NH2:23])=[CH:7][CH:6]=[N:5]1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 67265394N-(3-(2-methyl-2H-pyrazol-3-yl)-4-(2-methyl-2-nitropropoxy)phenyl)acetamide

生成物 1

HCID 672657453-(2-methyl-2H-pyrazol-3-yl)-4-(2-methyl-2-nitropropoxy)aniline収率 74%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

A solution of sodium hydroxide (70 mg, 1.74 mmol) in water (0.15 mL) was added to a suspension of N-(3-(2-methyl-2H-pyrazol-3-yl)-4-(2-methyl-2-nitropropoxy)phenyl)acetamide (84 mg, 0.29 mmol) in methanol (1 mL) and the mixture was stirred at 140° C. in a screw capped vial for 90 min. The mixture was allowed to cool to room temperature, and the solvent was removed under reduced pressure. The residue was partitioned between dichloromethane and water, the organic layer was dried with sodium sulfate, filtered and evaporated to dryness to afford the title compound (62 mg, 0.21 mmol, 74%) as a yellow oil which was used without further purification. LCMS m/z (%)=291.3 (M+H 98%).

後処理

  1. customcapped vial for 90 min
  2. temperatureto cool to room temperature
  3. customthe solvent was removed under reduced pressure
  4. customThe residue was partitioned between dichloromethane and water
  5. dry with materialthe organic layer was dried with sodium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-015f5109448749a09138f1ab7e446b8a
出典データセット
uspto-grants-2016_05
特許番号
US09328107B2

反応ノート

読み込み中…