Pyridine → HCID 86707263, 화합물

HRID 576045노트

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HRID 576045 반응식
N1C=CC=CC=1.CN(C1C=CC=CN=1)C.[F:16][C:17]1[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=1.[F:24][C:25]([F:42])([F:41])[C:26]([N:28]1[CH2:36][C:35]2[C:30](=[CH:31][CH:32]=[C:33]([S:37](Cl)(=[O:39])=[O:38])[CH:34]=2)[CH2:29]1)=[O:27]>C(Cl)(Cl)Cl>[F:16][C:17]1[CH:23]=[CH:22][C:20]([NH:21][S:37]([C:33]2[CH:34]=[C:35]3[C:30](=[CH:31][CH:32]=2)[CH2:29][N:28]([C:26](=[O:27])[C:25]([F:42])([F:24])[F:41])[CH2:36]3)(=[O:38])=[O:39])=[CH:19][CH:18]=1

참가 물질

6

반응물 4

HCID 1049PyridineHCID 97314-FluoroanilineHCID 218852-DimethylaminopyridineHCID 867072642,3-Dihydro-2-(2,2,2-trifluoroacetyl)-1H-isoindole-5-sulfonyl chloride

생성물 1

HCID 86707263HCID 86707263, 화합물수율 94.7%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Pyridine (2.57 mL, 31.9 mmol) and dimethylaminopyridine (195 mg, 1.59 mmol) were added to a solution of 4-fluoroaniline (1.86 g, 16.7 mmol) in chloroform (46 mL) at room temperature and the mixture was cooled in ice. 2-(Trifluoroacetyl)-2,3-dihydro-1 H-isoindole-5-sulfonyl chloride (5.00 g, 15.9 mmol) was added thereto and the mixture was warmed to room temperature and stirred for 15 hr. The reaction mixture was concentrated under reduced pressure and the residue was diluted with ethyl acetate. The mixture was washed with 1 mol/L hydrochloric acid and brine, the organic layer was dried over anhydrous magnesium sulfate, and then the desiccant was filtered off, followed by concentration under reduced pressure. The resulting residue was powdered with diethyl ether and collected by filtration to afford the title compound as a pale pink powder (5.85 g).

후처리

  1. temperaturethe mixture was cooled in ice
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. additionthe residue was diluted with ethyl acetate
  4. washThe mixture was washed with 1 mol/L hydrochloric acid and brine
  5. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  6. filtrationthe desiccant was filtered off
  7. concentrationfollowed by concentration under reduced pressure
  8. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-1a3473361da749be83dd5099d4e2951b
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09035059B2

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