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Water → Tert-butyl 2-(2-chloro-4-nitrophenoxy)ethyl(2,4-difluorobenzyl)carbamate

HRID 1019737
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HRID 1019737 반응식
[H-].[Na+].[F:3][C:4]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:5]=1[CH2:6][N:7]([CH2:15][CH2:16][OH:17])[C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11].[Cl:23][C:24]1[CH:25]=[C:26]([N+:31]([O-:33])=[O:32])[CH:27]=[CH:28][C:29]=1F.O>CN(C)C=O>[Cl:23][C:24]1[CH:25]=[C:26]([N+:31]([O-:33])=[O:32])[CH:27]=[CH:28][C:29]=1[O:17][CH2:16][CH2:15][N:7]([CH2:6][C:5]1[CH:18]=[CH:19][C:20]([F:22])=[CH:21][C:4]=1[F:3])[C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11]
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참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 676882-Chloro-1-fluoro-4-nitrobenzeneHCID 71294423tert-Butyl 2,4-difluorobenzyl(2-hydroxyethyl)carbamate

생성물 1

HCID 67468967Tert-butyl 2-(2-chloro-4-nitrophenoxy)ethyl(2,4-difluorobenzyl)carbamate수율 106.1%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
3회

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온도
-2.5 °C

실험 절차

Sodium hydride (0.101 g, 3.83 mmol, 95% in oil) was added to N,N-dimethyl formamide (20 mL) at −5 to 0° C. under nitrogen. The suspension was stirred for 10 minutes and to the resulting cooled mixture was added a solution of tert-butyl 2,4-difluorobenzyl(2-hydroxyethyl)carbamate (1.1 g, 4.21 mmol) in N,N-dimethylformamide (10 mL), maintaining the temperature at −5 to 0° C. during addition. The reaction mixture was stirred further for 20 minutes and then a solution of 3-chloro-4-fluoro-nitrobenzene (0.67 g, 3.83 mmol) in N,N-dimethyl formamide (10 mL), was added dropwise, maintaining the temperature in the range −5 to 0° C. The reaction mixture was allowed to warm to room temperature and stirred for 30 minutes. Water (300 mL) was then added to the reaction mixture and the resulting mixture was extracted with EtOAc (3×50 mL). The combined organic extracts were washed with brine (2×30 mL), dried (Na2SO4) and evaporated under reduced pressure. The residue was purified by column chromatography on neutral silica gel using 5-20% EtOAc in hexane to give the title compound (1.8 g, 60%).

후처리

  1. temperaturecooled mixture
  2. additionduring addition
  3. stirringThe reaction mixture was stirred further for 20 minutes
  4. temperaturemaintaining the temperature in the range −5 to 0° C
  5. temperatureto warm to room temperature
  6. stirringstirred for 30 minutes
  7. extractionthe resulting mixture was extracted with EtOAc (3×50 mL)
  8. washThe combined organic extracts were washed with brine (2×30 mL)
  9. dry with materialdried (Na2SO4)
  10. customevaporated under reduced pressure
  11. customThe residue was purified by column chromatography on neutral silica gel using 5-20% EtOAc in hexane

출처 및 근거

ORD 기록
ord-031bb321d0d24b209bd49008cfe1339c
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716287B2

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