Dimethyl Sulfate → HCID 300058, 화합물

HRID 984706

반응식

HRID 984706 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([Br:12])[CH:8]=2)[CH:3]=1.S(OC)(O[CH3:17])(=O)=O.C(OCC)(=O)C.[OH-].[Na+]>O1CCOCC1>[Br:12][C:7]1[CH:6]=[CH:5][C:4]2[C:9](=[CH:10][CH:11]=[C:2]([NH:1][CH3:17])[CH:3]=2)[CH:8]=1

참가 물질

6

반응물 4

HCID 6497Dimethyl SulfateHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 3484042-Amino-6-bromonaphthalene

생성물 1

HCID 300058HCID 300058, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of 2-amino-6-bromonaphthalene (2.0 g) in 1,4-dioxane (30 ml) was added dropwise with dimethyl sulfate (1300 μl) and stirred at room temperature for 46 hours. The reaction mixture was added with ethyl acetate (90 ml) and then added with 1 N aqueous sodium hydroxide (5 ml). This mixture was extracted with ethyl acetate (150 ml×3). The organic layer was washed with saturated brine and dried, and then the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography (hexane:ethyl acetate=15:1) to obtain the title compound (Intermediate 27, 152 mg).

후처리

  1. extractionThis mixture was extracted with ethyl acetate (150 ml×3)
  2. washThe organic layer was washed with saturated brine
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by flash column chromatography (hexane:ethyl acetate=15:1)

출처 및 근거

ORD 기록
ord-ab1d99d0d5f54fb4980e8525c0c08449
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06867320B2

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