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Ethanol → 3-Chloro-4-(tetrahydro-pyrimidin-2-on-1-yl)-benzoic acid

HRID 2222485
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반응식

HRID 2222485 반응식
[Cl:1][C:2]1[CH:3]=C([CH:7]=[CH:8][C:9]=1[N:10]1[CH2:15][CH2:14][CH2:13][NH:12][C:11]1=[O:16])C#N.[OH-:17].[Na+].[CH2:19]([OH:21])[CH3:20]>>[Cl:1][C:2]1[CH:3]=[C:20]([CH:7]=[CH:8][C:9]=1[N:10]1[CH2:15][CH2:14][CH2:13][NH:12][C:11]1=[O:16])[C:19]([OH:17])=[O:21]
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참가 물질

4

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 667319453-Chloro-4-(tetrahydro-pyrimidin-2-on-1-yl)-benzonitrile

생성물 1

HCID 643195303-Chloro-4-(tetrahydro-pyrimidin-2-on-1-yl)-benzoic acid

반응 조건

온도
100 °C

실험 절차

350 mg (1.49 mmol) 3-chloro-4-(tetrahydro-pyrimidin-2-on-1-yl)-benzonitrile are suspended in 5 ml of ethanol and combined with 2.0 ml of 10-molar aqueous sodium hydroxide solution. The mixture is stirred for one hour at 100° C. and then evaporated down i. vac. The aqueous residue is combined with ice, acidified with acetic acid and extracted with ethyl acetate. The combined organic phases are washed with water and sat. sodium chloride solution, dried over magnesium sulphate and evaporated down i. vac. The aqueous phase is acidified with 6-molar hydrochloric acid, extracted 5 times with ethyl acetate, the combined organic phases are washed with sat. sodium chloride solution, dried over magnesium sulphate and evaporated down i. vac.

후처리

  1. customevaporated down i
  2. extractionextracted with ethyl acetate
  3. washThe combined organic phases are washed with water and sat. sodium chloride solution
  4. dry with materialdried over magnesium sulphate
  5. customevaporated down i
  6. extractionextracted 5 times with ethyl acetate
  7. washthe combined organic phases are washed with sat. sodium chloride solution
  8. dry with materialdried over magnesium sulphate
  9. customevaporated down i

출처 및 근거

ORD 기록
ord-1e8f4cd6fdaa424bb52babf572b5d69d
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07371743B2

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