Sodium Acetate → HCID 58092097, 화합물

HRID 1873476

반응식

HRID 1873476 반응식
[C:1]([O-:4])(=[O:3])[CH3:2].[Na+].Br[CH2:7][C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([C:18]([NH:20][CH2:21][Si:22]([CH3:25])([CH3:24])[CH3:23])=[O:19])=[CH:10][CH:9]=1>CN(C=O)C.COC(C)(C)C>[C:1]([O:4][CH2:7][C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([C:18](=[O:19])[NH:20][CH2:21][Si:22]([CH3:25])([CH3:24])[CH3:23])=[CH:10][CH:9]=1)(=[O:3])[CH3:2]

참가 물질

5

반응물 2

HCID 517045Sodium AcetateHCID 580920724-(bromomethyl)-N-[(trimethylsilyl)methyl]naphthalene-1-carboxamide

생성물 1

HCID 58092097HCID 58092097, 화합물수율 55.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 15413tert-Butyl methyl ether용매

실험 절차

A mixed solution of sodium acetate (1.1 g), 4-(bromomethyl)-N-[(trimethylsilyl)methyl]naphthalen-1-carboxamide (2.5 g) in DMF (30 ml) was stirred for 3 hours at 70° C. The reaction mixture was returned to room temperature and diluted with t-butyl methyl ether. The mixture was washed with water and a saturated aqueous brine, subsequently dried over magnesium sulfate. After filtering the reaction mixture, the solvent was distilled off under reduced pressure, and the resulting mixture was purified by silica gel chromatography, to obtain (4{[(trimethylsilyl)methyl]carbamoyl}naphthalen-1-yl)methyl acetate (1.3 g).

후처리

  1. customwas returned to room temperature
  2. washThe mixture was washed with water
  3. dry with materiala saturated aqueous brine, subsequently dried over magnesium sulfate
  4. filtrationAfter filtering the reaction mixture
  5. distillationthe solvent was distilled off under reduced pressure
  6. customthe resulting mixture was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-6e07930c18cb41739054c5be1c4588c6
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304371B2

연결된 노트

불러오는 중…