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

HRID 2283726노트

반응식

HRID 2283726 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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. Anal. Calcd. for C6H6BrN3: C, 36.03; H, 3.02; N, 21.01. Found: C, 36.04; H, 2.86; N, 20.99.

후처리

  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

출처 및 근거

ORD 기록
ord-ab44c462b70c42ffa00b431485ffa35e
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09145410B2

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