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Potassium Carbonate → HCID 66742608, 화합물

HRID 449633
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HRID 449633 반응식
Br[C:2]1[C:3]([N+:8]([O-:10])=[O:9])=[N:4][CH:5]=[CH:6][N:7]=1.C([O-])([O-])=O.[K+].[K+].[CH3:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>O1CCOCC1>[CH3:17][N:18]1[CH2:23][CH2:22][N:21]([C:6]2[CH:5]=[N:4][C:3]([N+:8]([O-:10])=[O:9])=[CH:2][N:7]=2)[CH2:20][CH2:19]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 86662319HCID 86662319, 화합물

생성물 1

HCID 66742608HCID 66742608, 화합물수율 100%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
70 °C

실험 절차

In a 15 mL argon dried microwave reaction vial, was added bromonitropyrazine (300 mg, 1.47 mmol., Eq: 1.00) and K2CO3 (264 mg, 1.91 mmol., Eq: 1.3) under argon to give a light yellow slurry. N-methylpiperazine (192 mg, 212 μl, 1.91 mmol, Eq: 1.3) was added dropwise and the reaction mixture became an orange yellow thick slurry. Heated to 70° C. in an oil bath for 1.5 hrs then stirred at room temperature overnight. The reaction mixture was diluted with dioxane (10 mL), filtered through a fitted funnel and washed with DCM (10 mL). The combined filtrate and washes were concentrated to dryness to give a yellow solid (328 mg, yield 89%) which was used directly in the next step.

후처리

  1. customIn a 15 mL argon dried microwave reaction vial
  2. customto give a light yellow slurry
  3. filtrationfiltered through a fitted funnel
  4. washwashed with DCM (10 mL)
  5. concentrationThe combined filtrate and washes were concentrated to dryness

출처 및 근거

ORD 기록
ord-708ad224196948ceabdd15beb4ac33e3
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481540B2

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