Hydrochloric Acid → HCID 66984909, 화합물

HRID 1950776노트

반응식

HRID 1950776 반응식
Cl[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([CH3:13])[N:5]=[C:4]([S:14][CH3:15])[N:3]=1.[CH3:16][O:17][C:18]1[CH:19]=[C:20]([CH:22]=[C:23]([O:25][CH3:26])[CH:24]=1)[NH2:21].Cl>C(#N)C.C(OCC)(=O)C.C([O-])(O)=O.[Na+]>[CH3:26][O:25][C:23]1[CH:22]=[C:20]([NH:21][C:2]2[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([CH3:13])[N:5]=[C:4]([S:14][CH3:15])[N:3]=2)[CH:19]=[C:18]([O:17][CH3:16])[CH:24]=1

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 663013,5-DimethoxyanilineHCID 22225416Ethyl 4-chloro-6-methyl-2-(methylsulfanyl)pyrimidine-5-carboxylate

생성물 1

HCID 66984909HCID 66984909, 화합물수율 72.4%

시약·촉매·용매 3

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매

실험 절차

A 200 mL RB flask was charged with ethyl 4-chloro-6-methyl-2-(methylthio)pyrimidine-5-carboxylate (2.76 g, 11.1 mmol) in 40 mL acetonitrile. To the solution was added 3,5-dimethoxy aniline (1.784 g, 11.4 mmol), and conc. HCl solution (494 uL, 5.6 mmol), the reaction mixture was stirred at 60˜70° C. for 2 hours. The mixture was diluted with ethyl acetate and saturated aqueous NaHCO3 solution. It was stirred for an additional 5 minutes. The separated organic layer was dried over MgSO4, and condensed under reduced pressure yielding the residue. The residue was recrystallized from acetonitrile, dried under reduced pressure providing pale yellow solids (2.92 g, 72%). MS m/z: 364.1 (M+H)+.

후처리

  1. stirringIt was stirred for an additional 5 minutes
  2. dry with materialThe separated organic layer was dried over MgSO4, and condensed under reduced pressure
  3. customyielding the residue
  4. customThe residue was recrystallized from acetonitrile
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-aa5ec20b622c4f8298cd02e34237f04f
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404677B2

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