Sodium Chloride → [2-{2-Chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]acetic acid

HRID 493934ノート

反応式

HRID 493934 の反応式
[Cl:1][C:2]1[CH:19]=[C:18]([F:20])[C:17]([N:21]2[C:26](=[O:27])[CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[N:23]([CH3:32])[C:22]2=[O:33])=[CH:16][C:3]=1[O:4][C:5]1[CH:15]=[CH:14][CH:13]=[CH:12][C:6]=1[O:7][CH2:8][C:9]([O-:11])=[O:10].C(OCC)(=O)C.[Cl-].[Na+]>O1CCOCC1.Cl.O>[Cl:1][C:2]1[CH:19]=[C:18]([F:20])[C:17]([N:21]2[C:26](=[O:27])[CH:25]=[C:24]([C:28]([F:29])([F:30])[F:31])[N:23]([CH3:32])[C:22]2=[O:33])=[CH:16][C:3]=1[O:4][C:5]1[CH:15]=[CH:14][CH:13]=[CH:12][C:6]=1[O:7][CH2:8][C:9]([OH:11])=[O:10]

参加物

7

反応物 3

HCID 5234Sodium ChlorideHCID 8857Ethyl AcetateHCID 21933551HCID 21933551、化合物

生成物 1

HCID 21933550[2-{2-Chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]acetic acid

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

First, 0.4 g of methyl. [2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]acetate was dissolved in 4 ml of 1,4-dioxane, to which a mixed solution of 1 ml of concentrated hydrochloric acid and 1 ml of water was added under stirring, and the mixture was heated and stirred under reflux for 12 hours. The reaction mixture was then left for cooling, into which ice water was poured, and after addition of ethyl acetate and saturated aqueous sodium chloride solution, the mixture was subjected to phase separation. To the organic layer was added aqueous sodium hydrogencarbonate solution, and the mixture was subjected to phase separation. To the aqueous layer was added aqueous hydrochloric acid solution for acidification, to which ethyl acetate was added, and the mixture was subjected to phase separation. The organic layer was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate, and then concentrated to give 0.252 g of [2-{2-chloro-4-fluoro-5-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]phenoxy}phenoxy]acetic acid.

後処理

  1. additionwas added
  2. temperaturethe mixture was heated
  3. stirringstirred
  4. temperatureunder reflux for 12 hours
  5. waitThe reaction mixture was then left
  6. additionwas poured
  7. customthe mixture was subjected to phase separation
  8. additionTo the organic layer was added aqueous sodium hydrogencarbonate solution
  9. customthe mixture was subjected to phase separation
  10. additionTo the aqueous layer was added aqueous hydrochloric acid solution for acidification
  11. additionto which ethyl acetate was added
  12. customthe mixture was subjected to phase separation
  13. washThe organic layer was washed with saturated aqueous sodium chloride solution
  14. dry with materialdried over magnesium sulfate
  15. concentrationconcentrated

出典と根拠

ORDレコード
ord-9ee30756cef942deaae216871edd8d57
出典データセット
uspto-grants-2009_05
特許番号
US07538072B2

反応ノート

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