Potassium Carbonate → N-(5-bromo-3-methyl-pyridin-2-yl)-2-pyrrolidin-1-yl-acetamide

HRID 1916741

反応式

HRID 1916741 の反応式
[NH:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1.[Br:6][C:7]1[CH:8]=[C:9]([CH3:18])[C:10]([NH:13][C:14](=[O:17])[CH2:15]Cl)=[N:11][CH:12]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[Br:6][C:7]1[CH:8]=[C:9]([CH3:18])[C:10]([NH:13][C:14](=[O:17])[CH2:15][N:1]2[CH2:5][CH2:4][CH2:3][CH2:2]2)=[N:11][CH:12]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 31268PyrrolidineHCID 52228026n-(5-Bromo-3-methyl-pyridin-2-yl)-2-chloro-acetamide

生成物 1

HCID 67362705N-(5-bromo-3-methyl-pyridin-2-yl)-2-pyrrolidin-1-yl-acetamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

0.81 mL (9.9 mmol) pyrrolidine are added to a suspension of 2.37 g (9.0 mmol) N-(5-bromo-3-methyl-pyridin-2-yl)-2-chloro-acetamide and 2.49 g (18 mmol) K2CO3 in 22.5 mL DMF and the reaction mixture is stirred for 20 h at RT. It is diluted with water, extracted exhaustively with EtOAc, the combined organic phases are washed with water and dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is taken up in a little diisopropylether, cooled to 0° C., the crystals precipitated are suction filtered and dried in the air.

後処理

  1. extractionextracted exhaustively with EtOAc
  2. washthe combined organic phases are washed with water
  3. dry with materialdried over Na2SO4
  4. temperaturecooled to 0° C.
  5. customthe crystals precipitated
  6. filtrationare suction filtered
  7. customdried in the air

出典と根拠

ORDレコード
ord-c0b803486c1f41659abfeb3b7564a30c
出典データセット
uspto-grants-2013_12
特許番号
US08618132B2

関連ノート

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