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Water → tert-Butyl 4-(2-(2-chloropyridin-4-yloxy)ethyl)naphthalen-1-ylcarbamate

HRID 2069039
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반응식

HRID 2069039 반응식
[OH:1][CH2:2][CH2:3][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[CH:6][CH:5]=1.[H-].[Na+].[Cl:24][C:25]1[CH:30]=[C:29](F)[CH:28]=[CH:27][N:26]=1.O>CN(C=O)C>[Cl:24][C:25]1[CH:30]=[C:29]([O:1][CH2:2][CH2:3][C:4]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:18])([CH3:20])[CH3:19])=[CH:6][CH:5]=2)[CH:28]=[CH:27][N:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 27827922-Chloro-4-fluoropyridineHCID 68313879tert-Butyl 4-(2-hydroxyethyl)naphthalen-1-ylcarbamate

생성물 1

HCID 86659922tert-Butyl 4-(2-(2-chloropyridin-4-yloxy)ethyl)naphthalen-1-ylcarbamate수율 75.3%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
2회

실험 절차

To a degassed solution of tert-butyl 4-(2-hydroxyethyl)naphthalen-1-ylcarbamate (32) (0.64 g, 2.23 mmol) in DMF (10 mL) was added sodium hydride (0.267 g, 60% dispersion in mineral oil, 6.68 mmol) under nitrogen at 0° C. The solution was warmed to RT and was stirred for 30 min and then cooled to 0° C. To this mixture was added a solution of 2-chloro-4-fluoro-pyridine (0.381 g, 2.90 mmol) in DMF (5.0 mL) and the reaction mixture was warmed to RT and stirred for 16 hr. Water was added and the mixture was extracted with ethyl acetate. The ethyl acetate extract was washed with brine (3×), dried (MgSO4) and evaporated in vacuo. The residue was purified by flash column chromatography (SiO2, 0-40% ethyl acetate in isohexane, gradient elution) to afford the title compound (33) (0.67 g, 75%); m/z 399 (M+H)+, (ES+).

후처리

  1. temperaturecooled to 0° C
  2. temperaturethe reaction mixture was warmed to RT
  3. stirringstirred for 16 hr
  4. extractionthe mixture was extracted with ethyl acetate
  5. extractionThe ethyl acetate extract
  6. washwas washed with brine (3×)
  7. dry with materialdried (MgSO4)
  8. customevaporated in vacuo
  9. customThe residue was purified by flash column chromatography (SiO2, 0-40% ethyl acetate in isohexane, gradient elution)

출처 및 근거

ORD 기록
ord-bea0b31461f14fba9bfa6d992a63b2ff
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08299073B2

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