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Sodium Carbonate → HCID 58461049, 화합물

HRID 2173739
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HRID 2173739 반응식
Cl[C:2]1[C:7]([CH3:8])=[N:6][C:5]([CH3:9])=[CH:4][N:3]=1.[C:10]1([C:20]2[CH:25]=[CH:24][C:23](B(O)O)=[CH:22][CH:21]=2)[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:13]=[CH:12][CH:11]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl.O.C(#N)C>[CH3:8][C:7]1[C:2]([C:23]2[CH:24]=[CH:25][C:20]([C:10]3[C:19]4[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=4)[CH:13]=[CH:12][CH:11]=3)=[CH:21][CH:22]=2)=[N:3][CH:4]=[C:5]([CH3:9])[N:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 10340Sodium CarbonateHCID 116726802-Chloro-3,5-dimethylpyrazineHCID 441193994-(1-Naphthyl)phenylboronic Acid (contains varying amounts of Anhydride)

생성물 1

HCID 58461049HCID 58461049, 화합물수율 50%

시약·촉매·용매 3

HCID 6102075Dichlorobis(triphenylphosphine)palladium촉매
HCID 962
Water
용매
2회
HCID 6342Acetonitrile용매

실험 절차

First, into a recovery flask equipped with a reflux pipe were placed 0.74 g of 2-chloro-3,5-dimethylpyrazine, 1.29 g of 4-(1-naphthyl)phenylboronic acid, 0.55 g of sodium carbonate, 0.024 g of bis(triphenylphosphine)palladium(II)dichloride (abbreviation: Pd(PPh3)2Cl2), 10 mL of water, and 10 mL of acetonitrile, and the air in the flask was replaced with argon. This reaction container was irradiated with microwaves (2.45 GHz, 100 W) for 15 minutes, so that heating was performed. Then, the reaction container was cooled to 50° C. or less. Water was added to the reaction solution, and the organic layer was extracted with dichloromethane. The obtained organic layer was washed with water and dried with magnesium sulfate. The solution which had been dried was filtered. The solvent of this solution was distilled, and recrystallized using ethyl acetate, whereby Hdm1nppr, which is the pyrazine derivative to be produced, was obtained (as a white powder in 50% yield). Note that the microwave irradiation was performed using a microwave synthesis system (Discover, manufactured by CEM Corporation). The synthesis scheme of Step 1 is illustrated in the following (a-1).

후처리

  1. customFirst, into a recovery flask equipped with a reflux pipe
  2. customThis reaction container was irradiated with microwaves (2.45 GHz, 100 W) for 15 minutes
  3. temperatureso that heating
  4. temperatureThen, the reaction container was cooled to 50° C. or less
  5. extractionthe organic layer was extracted with dichloromethane
  6. washThe obtained organic layer was washed with water
  7. dry with materialdried with magnesium sulfate
  8. customThe solution which had been dried
  9. filtrationwas filtered
  10. distillationThe solvent of this solution was distilled
  11. customrecrystallized
  12. customto be produced
  13. customwas obtained (as a white powder in 50% yield)
  14. customNote that the microwave irradiation
  15. customa microwave synthesis system (Discover, manufactured by CEM Corporation)
  16. customThe synthesis scheme of Step 1

출처 및 근거

ORD 기록
ord-43ba3ceb736e4b339046cba7c0af6888
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056883B2

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