1-(6-Methylpyridin-3-yl)ethanamine → 4-Hydroxy-6-methyl-1-[1-(6-methyl-pyridin-3-yl)-ethyl]-1H-pyridin-2-one

HRID 2068714노트

반응식

HRID 2068714 반응식
[OH:1][C:2]1[CH:7]=[C:6]([CH3:8])O[C:4](=[O:9])[CH:3]=1.[CH3:10][C:11]1[N:16]=[CH:15][C:14]([CH:17]([NH2:19])[CH3:18])=[CH:13][CH:12]=1>O>[OH:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:19]([CH:17]([C:14]2[CH:15]=[N:16][C:11]([CH3:10])=[CH:12][CH:13]=2)[CH3:18])[C:4](=[O:9])[CH:3]=1

참가 물질

4

반응물 2

HCID 457910961-(6-Methylpyridin-3-yl)ethanamineHCID 546757574-Hydroxy-6-methyl-2-pyrone

생성물 1

HCID 596030954-Hydroxy-6-methyl-1-[1-(6-methyl-pyridin-3-yl)-ethyl]-1H-pyridin-2-one수율 17.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A stirred mixture of 4-Hydroxy-6-methyl-2-pyrone (1.394 g, 11.1 mmol) and 1-(6-Methyl-pyridin-3-yl)-ethylamine (1.806 g, 13.3 mmol) in water (18 ml) was boiled under reflux for 65 h. The mixture was cooled to ambient temperature and the supernatant liquid was decanted off to leave a dark semi-solid residue. This was triturated with ethyl acetate to give 4-Hydroxy-6-methyl-1-[1-(6-methyl-pyridin-3-yl)-ethyl]-1H-pyridin-2-one as a grey solid (475 mg) which was used in the next step without further purification. LC-MS m/z 245 [M+H]+ Rt=1.21 min.

후처리

  1. temperatureunder reflux for 65 h
  2. customthe supernatant liquid was decanted off
  3. customto leave a dark semi-solid residue
  4. customThis was triturated with ethyl acetate

출처 및 근거

ORD 기록
ord-2cad03700ab24716b4df40c9c073315c
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299065B2

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