Acetonitrile → HCID 86703140, 화합물

HRID 2204340노트

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HRID 2204340 반응식
[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][N:5]=[C:4](Cl)[CH:3]=1.S([O:16][CH3:17])(OC)(=O)=O.CC#N.C([O-])(O)=O.[Na+]>C(Cl)Cl>[Br:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][N:5]([CH3:4])[C:17](=[O:16])[CH:3]=1

참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 6497Dimethyl SulfateHCID 516892Sodium BicarbonateHCID 467387064-Bromo-2-chloro-5-methoxypyridine

생성물 1

HCID 86703140HCID 86703140, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 4-bromo-2-chloro-5-methoxypyridine [1020253-15-9] (1 g, 4.5 mmol) in dimethyl sulfate (1.9 mL, 19.5 mmol) was stirred at 120° C. for 16 h in a sealed tube. After cooling to rt, CH3CN and a saturated aqueous NaHCO3 solution were added and the mixture was stirred at rt over the weekend. CH2Cl2 was added and the phases were separated. The organic layer was dried (Na2SO4), filtered and concentrated to give the title compound as a white powder. ESI-MS: tR=0.57 min; [M+H]+ 218/220 (LC-MS 1).

후처리

  1. customthe phases were separated
  2. dry with materialThe organic layer was dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-79572fbb1f974f1b9cb763aac7064f17
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09365576B2

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