Hydrochloric Acid → 1-(1,3-dimethyl-1H-pyrazol-4-yl)ethan-1-one

HRID 2274974

反応式

HRID 2274974 の反応式
[CH3:1][N:2]([CH:7]=[C:8]([C:12](=[O:14])[CH3:13])[C:9](=O)[CH3:10])[N:3]=C(C)C.Cl>C(O)C.O>[CH3:1][N:2]1[CH:7]=[C:8]([C:12](=[O:14])[CH3:13])[C:9]([CH3:10])=[N:3]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 236352723-((1-Methyl-2-(propan-2-ylidene)hydrazinyl)methylene)pentane-2,4-dione

生成物 1

HCID 8439771-(1,3-dimethyl-1H-pyrazol-4-yl)ethan-1-one

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

3-((1-methyl-2-(propan-2-ylidene)hydrazinyl)methylene)pentane-2,4-dione (Preparation 3, 9.1 g) was dissolved in Ethanol (20 mL) and treated with 1M Hydrogen chloride in Water (20 mL). the reaction solution was stirred at room temperature for 15 minutes. The reaction solution was then concentrated under vacuum with a rotavap to approximately 20 mL total volume. The reaction solution was then treated with saturated aqueous sodium bicarbonate (45 mL), and extracted with methylene chloride (4×50 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo afford the title compound as a light orange solid. (6.2 g, 97%).

後処理

  1. concentrationThe reaction solution was then concentrated under vacuum with a rotavap to approximately 20 mL total volume
  2. additionThe reaction solution was then treated with saturated aqueous sodium bicarbonate (45 mL)
  3. extractionextracted with methylene chloride (4×50 mL)
  4. dry with materialThe combined organic extracts were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4acac7276a8a47d58d29aa45aab0cef8
出典データセット
uspto-grants-2015_09
特許番号
US09126999B2

関連ノート

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