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Trifluoroacetic acid → HCID 18695982, 화합물

HRID 1870617
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HRID 1870617 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:18]3[CH:19]=[CH:20][C:21]([F:23])=[CH:22][C:17]=3[N:16]([CH2:24][C:25]([F:28])([F:27])[F:26])[C:15]2=[O:29])[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)(Cl)Cl>[F:23][C:21]1[CH:20]=[CH:19][C:18]2[N:14]([CH:11]3[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]3)[C:15](=[O:29])[N:16]([CH2:24][C:25]([F:27])([F:28])[F:26])[C:17]=2[CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 186959641-Tert-butoxycarbonyl-4-(5-fluoro-3-(2,2,2-trifluoroethyl)-2-oxo-1-benzimidazolinyl)piperidine

생성물 1

HCID 18695982HCID 18695982, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 1-tert-butoxycarbonyl-4-(5-fluoro-3-(2,2,2-trifluoroethyl)-2-oxo-1-benzimidazolinyl)piperidine (4.17 g, 10 mmol.) in chloroform (50 mL) containing trifluoroacetic acid (5.5 mL) was stirred at room temp. under an inert atmosphere for 6-12 hours until reaction was complete. The solvent and excess TFA were removed and the residue redissolved in chloroform. This solution was washed with Na2CO3 /NaOH solution. The organic layer was dried (Na2SO4), filtered through a pad of charcoal, and the solvent evaporated to give 4-(5-fluoro-3-(2,2,2-trifluoroethyl)-2-oxo-1-benzimidazolinyl)piperidine as a viscous oil which was used as is. A sample of this material was converted to the HCl salt and after crystallization from methanol gave a white solid, mp: >280° C.

후처리

  1. customThe solvent and excess TFA were removed
  2. dissolutionthe residue redissolved in chloroform
  3. washThis solution was washed with Na2CO3 /NaOH solution
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. filtrationfiltered through a pad of charcoal
  6. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-e2c2ab1e3a444c6fade92af0dea895ed
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06096763

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