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

HRID 1183911노트

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HRID 1183911 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
140 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-992bbd7e09bc4719a31d59956c829e62
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08664258B2

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