Sodium hydride → HCID 68580572, 화합물

HRID 886976노트

반응식

HRID 886976 반응식
[CH2:1]([N:8]([CH2:20][CH2:21][OH:22])[C:9](=[O:19])[C:10]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]([Br:17])[C:11]=1F)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+]>CN(C)C=O>[CH2:1]([N:8]1[C:9](=[O:19])[C:10]2[CH:15]=[CH:14][C:13]([F:16])=[C:12]([Br:17])[C:11]=2[O:22][CH2:21][CH2:20]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 68578370HCID 68578370, 화합물

생성물 1

HCID 68580572HCID 68580572, 화합물수율 75%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of N-benzyl-3-bromo-2,4-difluoro-N-(2-hydroxyethyl)benzamide (4.57 g, 12.3 mmol) in N,N-dimethylformamide (60 ml) was added under ice-cooling sodium hydride (60%, 593 mg, 14.8 mmol), and the mixture was stirred for 2 hr. The reaction mixture was poured into ice water, and the mixture was extracted with ethyl acetate. The extract was washed with water and brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1) to give the desired product (3.23 g, 75.0%) as an oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1)

출처 및 근거

ORD 기록
ord-383382fc6caf4a6ba285e13632b69d0a
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08247403B2

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