Potassium Carbonate → HCID 66798808, 화합물

HRID 1193396노트

반응식

HRID 1193396 반응식
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([O:9][CH3:10])[N:3]=1.[CH3:11][N:12]([CH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1)[C:13](=[O:22])[O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[CH3:10][O:9][C:4]1[N:3]=[C:2]([N:26]2[CH2:25][CH2:24][CH:23]([N:12]([CH3:11])[C:13](=[O:22])[O:14][CH2:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:28][CH2:27]2)[CH:7]=[C:6]([CH3:8])[N:5]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 134258364-Chloro-2-methoxy-6-methylpyrimidineHCID 18677746Benzyl methyl(piperidin-4-yl)carbamate

생성물 1

HCID 66798808HCID 66798808, 화합물수율 71%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 4-chloro-2-methoxy-6-methylpyrimidine (300 mg, 1.8987 mmol, 1 eq), benzyl methyl(piperidin-4-yl)carbamate (stage 3 AMN-52) (470 mg, 1.8987 mmol, 1 eq) and K2CO3 (523 mg, 3.796 mmol, 2 eq) in acetone (10 ml) was refluxed for 16 h. When the reaction was complete according to TLC monitoring, filtration over Celite was carried out and the filtrate was concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel, 2% methanol/dichloromethane). The desired product was in the form of a light-yellow solid. Yield: 71% (500 mg, 1.3513 mmol)

후처리

  1. temperaturewas refluxed for 16 h
  2. filtrationWhen the reaction was complete according to TLC monitoring, filtration over Celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe crude product was purified by column chromatography (silica gel, 2% methanol/dichloromethane)

출처 및 근거

ORD 기록
ord-c650793b5ff1464aa194293de14e18b8
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680159B2

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