Trifluoroacetic acid → 3-chloro-4-hydroxy-2'-(2-(2-hydroxypropan-2-yl)pyrimidin-4-yl)-5',6-dimethyl-2H-[1,4'-bipyridin]-2-one

HRID 2199522노트

반응식

HRID 2199522 반응식
[Cl:1][C:2]1[C:3](=[O:36])[N:4]([C:19]2[C:24]([CH3:25])=[CH:23][N:22]=[C:21]([C:26]3[CH:31]=[CH:30][N:29]=[C:28]([C:32]([OH:35])([CH3:34])[CH3:33])[N:27]=3)[CH:20]=2)[C:5]([CH3:18])=[CH:6][C:7]=1[O:8]CC1C=CC(OC)=CC=1.FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:3](=[O:36])[N:4]([C:19]2[C:24]([CH3:25])=[CH:23][N:22]=[C:21]([C:26]3[CH:31]=[CH:30][N:29]=[C:28]([C:32]([OH:35])([CH3:33])[CH3:34])[N:27]=3)[CH:20]=2)[C:5]([CH3:18])=[CH:6][C:7]=1[OH:8]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 866993073-chloro-2'-(2-(2-hydroxypropan-2-yl)pyrimidin-4-yl)-4-((4-methoxybenzyl)oxy)-5',6-dimethyl-2H-[1,4'-bipyridin]-2-one

생성물 1

HCID 866993063-chloro-4-hydroxy-2'-(2-(2-hydroxypropan-2-yl)pyrimidin-4-yl)-5',6-dimethyl-2H-[1,4'-bipyridin]-2-one수율 87.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-chloro-2′-(2-(2-hydroxypropan-2-yl)pyrimidin-4-yl)-4-((4-methoxybenzyl)oxy)-5′,6-dimethyl-2H-[1,4′-bipyridin]-2-one (2.53 g, 5.00 mmol) in dichloromethane (20 mL) was added trifluoroacetic acid (1.0 mL). The solution was stirred for several hours at room temperature. The solution was concentrated, diluted with water and extracted several times with ethyl acetate. The combined organic layers were dried (MgSO4), filtered and concentrated to provide 1.7 g of the title compound: MS (M+H) 388.

후처리

  1. concentrationThe solution was concentrated
  2. additiondiluted with water
  3. extractionextracted several times with ethyl acetate
  4. dry with materialThe combined organic layers were dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ec934604618c499ba2eac55f7f066c17
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359300B2

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