Potassium Carbonate → HCID 14793344, 화합물

HRID 570185

반응식

HRID 570185 반응식
[CH2:1]([O:3][C:4]([C:6]1[N:7]([CH3:15])[N:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)=[O:5])[CH3:2].C([O-])([O-])=O.[K+].[K+].[Br:22]Br>C(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[N:7]([CH3:15])[N:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:10]=1[Br:22])=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 24408BromineHCID 2799344ethyl 3-(tert-butyl)-1-methyl-1H-pyrazole-5-carboxylate

생성물 1

HCID 14793344HCID 14793344, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of 5-tert-butyl-2-methyl-pyrazole-3-carboxylic acid ethyl ester (2.00 g, 9.51 mmol) and K2CO3 (3.94 g, 28.5 mmol) in DCM (120 mL), in the dark, was added Br2 (1.46 mL, 28.5 mmol) slowly under Ar. After stirring at room temperature for 3 h under Ar, the resulting mixture was quenched with saturated aqueous Na2S2O3 (50 mL). The organic layer was separated and washed with H2O (50 mL) and brine (50 mL), then dried with Na2SO4. Removal of the solvent under reduced pressure yielded a white solid. 1H-NMR (400 MHz, CDCl3) δ: 4.40 (q, J=7.1 Hz, 2H), 4.08 (s, 3H), 1.43 (t, J=7.1 Hz, 3H), 1.42 (m, 9H). Mass Spectrum (LCMS, ESI pos.) Calculated For C11H17BrN2O2: 289.1 (M+H), Measured: 289.1.

후처리

  1. customthe resulting mixture was quenched with saturated aqueous Na2S2O3 (50 mL)
  2. customThe organic layer was separated
  3. washwashed with H2O (50 mL) and brine (50 mL)
  4. dry with materialdried with Na2SO4
  5. customRemoval of the solvent under reduced pressure
  6. customyielded a white solid

출처 및 근거

ORD 기록
ord-6068e5464a65454e84925cd59103ee60
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09023846B2

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