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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 2214377
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인쇄 미리보기

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HRID 2214377 반응식
[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]
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참가 물질

7

반응물 3

HCID 5234Sodium ChlorideHCID 8857Ethyl AcetateHCID 21933551HCID 21933551, 화합물

생성물 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

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매
HCID 962
Water
용매
HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9088c5c4ce93462ab73e8434ba131c6c
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07109148B2

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