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

HRID 13521

반응식

HRID 13521 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-af128e83c6f54f678c93c97cdc93799f
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728010B2

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