Potassium Carbonate → tert-butyl 2-(5'-bromo-3,4,5,6-tetrahydro-2H-[1,2]bipyridinyl-4-yl)ethylcarbamate

HRID 1019694

反応式

HRID 1019694 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][N:3]=1.[NH:9]1[CH2:14][CH2:13][CH:12]([CH2:15][CH2:16][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:11][CH2:10]1.C(=O)([O-])[O-].[K+].[K+].C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[Br:8][C:5]1[CH:6]=[CH:7][C:2]([N:9]2[CH2:14][CH2:13][CH:12]([CH2:15][CH2:16][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:22])([CH3:21])[CH3:23])[CH2:11][CH2:10]2)=[N:3][CH:4]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 693532,5-DibromopyridineHCID 516892Sodium BicarbonateHCID 15018494-(2-Aminoethyl)piperidine, 4-BOC protected

生成物 1

HCID 66661183tert-butyl 2-(5'-bromo-3,4,5,6-tetrahydro-2H-[1,2]bipyridinyl-4-yl)ethylcarbamate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
130 °C

実験手順

10.37 g (43.80 mmol) of 2,5-dibromopyridine, 10.00 g (43.80 mmol) of tert-butyl 2-piperidin-4-ylethylcarbamate and 6.05 g (43.80 mmol) of potassium carbonate are placed in an autoclave. The mixture is then heated at 130° C. for 12 hours. The reaction mixture is allowed to cool to room temperature and then taken up in chloroform and saturated aqueous sodium hydrogen carbonate solution. The aqueous phase is separated out and extracted twice with chloroform, and the combined organic phases are washed with saturated aqueous sodium chloride solution and dried over sodium sulfate, and the filtrate is concentrated under reduced pressure.

後処理

  1. temperatureto cool to room temperature
  2. customThe aqueous phase is separated out
  3. extractionextracted twice with chloroform
  4. washthe combined organic phases are washed with saturated aqueous sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. concentrationthe filtrate is concentrated under reduced pressure

出典と根拠

ORDレコード
ord-dab2bd828e60411a9ec5e24385c50ac9
出典データセット
uspto-grants-2014_05
特許番号
US08716289B2

関連ノート

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