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Sodium hydride → HCID 86705188, 화합물

HRID 2401283
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HRID 2401283 반응식
[H-].[Na+].[CH3:3][CH:4]([CH:6]1[CH2:10][N:9]([C:11]2[CH:12]=[N:13][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:15][CH:16]=2)[C:8](=[O:21])[NH:7]1)[CH3:5].Cl[CH2:23][C:24]([NH:26][C:27]1[CH:32]=[CH:31][CH:30]=[C:29]([C:33]([F:36])([F:35])[F:34])[CH:28]=1)=[O:25].C(=O)([O-])O.[Na+]>CN(C=O)C.O>[O:21]=[C:8]1[N:9]([C:11]2[CH:12]=[N:13][C:14]([C:17]([F:19])([F:18])[F:20])=[CH:15][CH:16]=2)[CH2:10][CH:6]([CH:4]([CH3:3])[CH3:5])[N:7]1[CH2:23][C:24]([NH:26][C:27]1[CH:32]=[CH:31][CH:30]=[C:29]([C:33]([F:34])([F:35])[F:36])[CH:28]=1)=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 24758Sodium hydrideHCID 516892Sodium BicarbonateHCID 7367442-Chloro-N-(3-(trifluoromethyl)phenyl)acetamideHCID 86705189HCID 86705189, 화합물

생성물 1

HCID 86705188HCID 86705188, 화합물수율 91%

시약·촉매·용매 2

HCID 962Water
용매
HCID 6228Dimethylformamide용매

실험 절차

Sodium hydride (60%, 22 mg) was added to a solution of 4-(propan-2-yl)-1-[6-(trifluoromethyl)pyridin-3-yl]imidazolidin-2-one (50 mg) in DMF (1.5 mL), and the mixture was stirred at room temperature for 15 min. After 2-chloro-N-[3-(trifluoromethyl)phenyl]acetamide (52 mg) was added thereto, the resulting mixture was stirred at room temperature for 21 hr. Water and saturated aqueous sodium hydrogen carbonate solution were added to the reaction mixture, followed by extraction with chloroform. The organic layer was separated out by phase separation cartridge and concentrated under reduced pressure. The residue was purified by column chromatography (NH cartridge, and silica gel cartridge, hexane/ethyl acetate) and preparative HPLC to afford the title compound (79 mg).

후처리

  1. stirringthe resulting mixture was stirred at room temperature for 21 hr
  2. extractionfollowed by extraction with chloroform
  3. customThe organic layer was separated out by phase separation cartridge
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography (NH cartridge, and silica gel cartridge, hexane/ethyl acetate) and preparative HPLC

출처 및 근거

ORD 기록
ord-1a4bdb6ce4f442e387e5c35bbf43fcb5
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08796272B2

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