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

HRID 2094262
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인쇄 미리보기

반응식

HRID 2094262 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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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-e68696898e09404391280b8dcd7bb4be
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445525B2

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