Bromine → HCID 21837347, 화합물

HRID 725277노트

반응식

HRID 725277 반응식
[Br:1]Br.[CH2:3]([C:5]1[CH:9]=[C:8]([CH2:10][CH3:11])[N:7]([C:12]2[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=2[CH3:20])[N:6]=1)[CH3:4]>C(O)(=O)C>[Br:1][C:9]1[C:5]([CH2:3][CH3:4])=[N:6][N:7]([C:12]2[C:17]([CH3:18])=[CH:16][C:15]([CH3:19])=[CH:14][C:13]=2[CH3:20])[C:8]=1[CH2:10][CH3:11]

참가 물질

4

반응물 2

HCID 24408BromineHCID 218373383,5-Diethyl-1-(2,4,6-trimethylphenyl)-1H-pyrazole

생성물 1

HCID 21837347HCID 21837347, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

A solution of 6.4 g (0.04 mol) of bromine in 20 mL of glacial acetic acid was added dropwise to a stirred solution of 9.00 g (37 mmol) of 3,5-diethyl-1-(2,4,6-trimethylphenyl)pyrazole in 100 mL of glacial acetic acid. After 1 hour at room temperature, the acetic acid was evaporated under reduced pressure and the residues were dissolved in ethyl acetate. This solution was washed with saturated sodium bicarbonate to remove residual acetic acid, dried with brine and magnesium sulfate, and was concentrated on the rotovap. The product was a tan solid (10.26 g, purification. 1H-NMR(CDCl3):0.92 (3H, t, J=7), 1.15 (3H, t, J=7), 1.86 (6H, s), 2.24 (3H, s), 2.32 (2H, q, J=7), 2.60 (2H, q, J=7), 6.82 (2H, s).

후처리

  1. customthe acetic acid was evaporated under reduced pressure
  2. dissolutionthe residues were dissolved in ethyl acetate
  3. washThis solution was washed with saturated sodium bicarbonate
  4. customto remove residual acetic acid
  5. dry with materialdried with brine and magnesium sulfate
  6. concentrationwas concentrated on the rotovap
  7. custom10.26 g, purification

출처 및 근거

ORD 기록
ord-5b268863696546f9aebf52fa3e9a5e27
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705646

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