Benzhydrylamine → 3-(Benzhydrylamino)-3-methylbutan-2-one

HRID 1437245노트

반응식

HRID 1437245 반응식
Br[C:2]([CH3:7])([CH3:6])[C:3](=[O:5])[CH3:4].[CH:8]([NH2:21])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>CO.C(N(CC)CC)C>[CH:8]([NH:21][C:2]([CH3:7])([CH3:6])[C:3](=[O:5])[CH3:4])([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

5

반응물 2

HCID 7036BenzhydrylamineHCID 3449113-Bromo-3-methyl-2-butanone

생성물 1

HCID 103783013-(Benzhydrylamino)-3-methylbutan-2-one

시약·촉매·용매 2

HCID 887Methanol용매HCID 8471Triethylamine용매

실험 절차

To the above-obtained 3-bromo-3-methylbutan-2-one (5.88 g) in methanol (30 mL), benzhydrylamine (5.0 mL) and triethylamine (7.5 mL) were added. The resultant mixture was stirred at 70° C. for 24 hours, and then cooled in air. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was sequentially washed with saturated aqueous sodium hydrogencarbonate and saturated brine, and then dried over magnesium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure, and to the solid, diethyl ether was added, and then insoluble matter was removed by filtration. The mother liquid was brought to the dryness under reduced pressure. The residue was purified through silica gel column chromatography (hexane-ethyl acetate), to thereby give 3-(benzhydrylamino)-3-methylbutan-2-one as an oily product (3.3 g, 34%).

후처리

  1. temperaturecooled in air
  2. customThe reaction mixture was partitioned between water and ethyl acetate
  3. washThe organic layer was sequentially washed with saturated aqueous sodium hydrogencarbonate and saturated brine
  4. dry with materialdried over magnesium sulfate anhydrate
  5. filtrationfollowed by filtration
  6. customThe solvent was evaporated under reduced pressure
  7. additionto the solid, diethyl ether was added
  8. custominsoluble matter was removed by filtration
  9. customThe residue was purified through silica gel column chromatography (hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-1ba1062def9a4ca19e6b16ec356f0ab2
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07622471B2

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