Potassium Carbonate → HCID 66798808、化合物

HRID 1193396ノート

反応式

HRID 1193396 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 66798808HCID 66798808、化合物収率 71%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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)

後処理

  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)

出典と根拠

ORDレコード
ord-c650793b5ff1464aa194293de14e18b8
出典データセット
uspto-grants-2014_03
特許番号
US08680159B2

反応ノート

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