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Potassium Carbonate → methyl 3-methyl-1-(1-phenylethyl)-1H-pyrazole-4-carboxylate

HRID 2206452
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HRID 2206452 반응식
[CH3:1][C:2]1[C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][NH:4][N:3]=1.Br[CH:12]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:13].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:1][C:2]1[C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][N:4]([CH:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH3:13])[N:3]=1.[CH3:1][C:2]1[N:3]([CH:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH3:13])[N:4]=[CH:5][C:6]=1[C:7]([O:9][CH3:10])=[O:8]
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참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 11454(1-Bromoethyl)benzeneHCID 178498883HCID 178498883, 화합물

생성물 2

HCID 89740139methyl 3-methyl-1-(1-phenylethyl)-1H-pyrazole-4-carboxylate수율 19%HCID 89740272methyl 5-methyl-1-(1-phenylethyl)-1H-pyrazole-4-carboxylate수율 16%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

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온도
20 °C

실험 절차

To a solution of methyl 3-methyl-1H-pyrazole-4-carboxylate (280 mg, 2 mmol) in N, N-dimethylformamide (30 mL) was added (1-bromoethyl)benzene (0.37 g, 2 mmol) and potassium carbonate (0.55 g, 4 mmol). The mixture was stirred at 20° C. and stirred for 12 hours. The solvent was evaporated in vacuo and the residue was purified by CXTH (Column: Dsisol, 10 μM, C18, 250 mm*50 mm; Mobile: acetonitrile (0.1% formic acid)-water (0.1% formic acid), acetonitrile from 30% to 70% in 80 minutes; oven: 20° C.; flow rate: 50 ml/minute, wavelength: 214 nm) to give methyl 3-methyl-1-(1-phenylethyl)-1H-pyrazole-4-carboxylate (90 mg, 19%) and methyl 5-methyl-1-(1-phenylethyl)-1H-pyrazole-4-carboxylate (80 mg, 16%). The product was used directly in the following reaction. LRMS (M+H+) m/z: calcd 244.12. found 244.

후처리

  1. stirringstirred for 12 hours
  2. customThe solvent was evaporated in vacuo
  3. customthe residue was purified by CXTH (Column: Dsisol, 10 μM, C18, 250 mm*50 mm; Mobile: acetonitrile (0.1% formic acid)-water (0.1% formic acid), acetonitrile from 30% to 70% in 80 minutes; oven: 20° C.; flow rate: 50 ml/minute, wavelength: 214 nm)

출처 및 근거

ORD 기록
ord-8ad99ca8658f488f80ed978af0bd146c
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09371331B2

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