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Sodium hydride → HCID 86695952, 화합물

HRID 870963
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HRID 870963 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][N:11]=[C:10]([CH3:14])[C:9]=2[CH2:15][OH:16])=[C:4](F)[CH:3]=1.[H-].[Na+]>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[C:8]3[C:9](=[C:10]([CH3:14])[N:11]=[CH:12][CH:13]=3)[CH2:15][O:16][C:4]=2[CH:3]=1
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참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 86695951(4-(4-Chloro-2-fluorophenyl)-2-methylpyridin-3-yl)methanol

생성물 1

HCID 86695952HCID 86695952, 화합물수율 170.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (4-(4-chloro-2-fluorophenyl)-2-methylpyridin-3-yl)methanol (70 mg, 0.278 mmol) in tetrahydrofuran (3 mL) at 0° C. was added NaH (33.4 mg, 0.834 mmol) portionwise. The solution was allowed to warm to room temperature and stirred for 5 h. The reaction mixture was quenched with ice cold water and diluted with EtOAc (15 mL). The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure to afford 8-chloro-4-methyl-5H-chromeno[3,4-c]pyridine (0.11 g, 0.475 mmol, 73% yield) as a brown solid. LCMS (ESI) m/e 232.00 [(M+H)+, calcd for C13H12ClNO 232.01]; LC/MS retention time (Method G): tR=1.00 min.

후처리

  1. customThe reaction mixture was quenched with ice cold water
  2. additiondiluted with EtOAc (15 mL)
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6587e57644534bd380ce99d36e4d3529
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969564B2

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