Bromine → 4-bromo-1,5-dimethyl-1H-pyrazole-3-carbonitrile

HRID 1984325ノート

反応式

HRID 1984325 の反応式
[Br:1]Br.C([O-])(=O)C.[K+].[CH3:8][N:9]1[C:13]([CH3:14])=[CH:12][C:11]([C:15]#[N:16])=[N:10]1.S([O-])(O)=O.[Na+]>C(O)(=O)C>[Br:1][C:12]1[C:11]([C:15]#[N:16])=[N:10][N:9]([CH3:8])[C:13]=1[CH3:14]

参加物

6

反応物 4

HCID 24408BromineHCID 517044Potassium AcetateHCID 122118911,5-dimethyl-1H-pyrazole-3-carbonitrileHCID 23665763Sodium Bisulfite

生成物 1

HCID 669589664-bromo-1,5-dimethyl-1H-pyrazole-3-carbonitrile

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

A solution of bromine (5.1 g, 32 mmol) in acetic acid (10 mL) was added dropwise to a solution of potassium acetate (3.9 g, 40 mmol) and 1,5-dimethyl-1H-pyrazole-3-carbonitrile in acetic acid (50 mL). Following the addition, the reaction was stirred for 30 minutes. Saturated aqueous sodium hydrogensulfite was added, and the mixture was stirred until it became colorless. The volatiles were removed under reduced pressure, and the residue was stirred with water to form a solid. The solid was isolated by filtration, washed with water, and recrystallized from ethanol and then from hexane to provide 2.5 g of 4-bromo-1,5-dimethyl-1H-pyrazole-3-carbonitrile as colorless needles, mp 92-94° C.

後処理

  1. additionthe addition
  2. stirringthe mixture was stirred until it
  3. customThe volatiles were removed under reduced pressure
  4. stirringthe residue was stirred with water
  5. customto form a solid
  6. customThe solid was isolated by filtration
  7. washwashed with water
  8. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-a9dfe3af2d7842e6aafa4a95ce28418f
出典データセット
uspto-grants-2009_06
特許番号
US07544697B2

反応ノート

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