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 2199522ノート

反応式

HRID 2199522 の反応式
[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]

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ec934604618c499ba2eac55f7f066c17
出典データセット
uspto-grants-2016_06
特許番号
US09359300B2

反応ノート

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