Dimethylamine → 4-chloro-N,N-dimethylpyridine-2-carboxamide

HRID 13521

反応式

HRID 13521 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8](Cl)=[O:9])[CH:3]=1.[CH2:11]([N:13](CC)[CH2:14]C)C.CNC>ClCCl>[CH3:11][N:13]([CH3:14])[C:8]([C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[CH:6][N:5]=1)=[O:9]

参加物

5

反応物 3

HCID 674DimethylamineHCID 8471TriethylamineHCID 110951464-chloropyridine-2-carbonyl Chloride

生成物 1

HCID 49622524-chloro-N,N-dimethylpyridine-2-carboxamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 4-chloro-pyridine-2-carbonyl chloride (1 eq) in dichloromethane was cooled to 0° C., whereupon triethylamine (2 eq) was added followed by dimethylamine (2 eq, 2M solution in THF). The solution was allowed to warm to room temperature and let stir overnight. It was then washed with 1M NaOH. The separated organic layer is dried over MgSO4, filtered, and concentrated to yield the desired product. HPLC, 1.82 min; MS: MH+=185.6

後処理

  1. additionwas added
  2. washIt was then washed with 1M NaOH
  3. dry with materialThe separated organic layer is dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-af128e83c6f54f678c93c97cdc93799f
出典データセット
uspto-grants-2010_06
特許番号
US07728010B2

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