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Sodium Carbonate → HCID 58305606, 화합물

HRID 2362249
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HRID 2362249 반응식
P(Cl)(Cl)(Cl)=O.[Br:6][C:7]1[N:8]([C:12]2[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[CH:14][C:13]=2[CH3:20])[CH:9]=[CH:10][CH:11]=1.[C:21](=O)([O-])[O-:22].[Na+].[Na+]>CN(C=O)C>[Br:6][C:7]1[N:8]([C:12]2[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[CH:14][C:13]=2[CH3:20])[C:9]([CH:21]=[O:22])=[CH:10][CH:11]=1
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참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 58305731HCID 58305731, 화합물

생성물 1

HCID 58305606HCID 58305606, 화합물수율 58%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

DMF (0.1 mL) was added to phosphorus oxychloride (0.5 mL, 5.2 mmol) at 0° C., and the mixture was stirred at room temperature for 1.5 h. At 0° C., a solution of compound 50B (100 mg. 0.36 mmol) in DMF (2 mL) was added, and the resultant mixture was stirred at room temperature for 30 min. The reaction mixture was poured into ice-water, adjusted to pH=8 with saturated aqueous sodium carbonate solution, and extracted with ethyl acetate (10 mL×3). The combined organic layers were washed with brine (20 mL×2), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by preparative TLC to afford 50C (60 mg, yield 58%).

후처리

  1. extractionextracted with ethyl acetate (10 mL×3)
  2. washThe combined organic layers were washed with brine (20 mL×2)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by preparative TLC

출처 및 근거

ORD 기록
ord-84d6441963eb483bac1ca471968f8cb6
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691816B2

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