Water → 1-{6-[Ethyl-(2-hydroxylethyl)-amino]-2-naphthyl}ethanone

HRID 431434

반응식

HRID 431434 반응식
O[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([C:12](=[O:14])[CH3:13])[CH:6]=[CH:5]2.[CH2:15]([NH:17][CH2:18][CH2:19][OH:20])[CH3:16].O>C(OCC)(=O)C>[CH2:15]([N:17]([CH2:18][CH2:19][OH:20])[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([C:12](=[O:14])[CH3:13])[CH:6]=[CH:5]2)[CH3:16]

참가 물질

5

반응물 3

HCID 962Water2회HCID 80722-(Ethylamino)ethanolHCID 826311-(6-Hydroxy-2-naphthyl)ethan-1-one

생성물 1

HCID 153748091-{6-[Ethyl-(2-hydroxylethyl)-amino]-2-naphthyl}ethanone수율 12%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1-(6-hydroxy-2-naphthyl)ethanone (744 mg, 3.92 mmol), sodium hydrogen sulfate(IV) (1.66 g, 16 mmol), 2-ethylaminoethanol (2 mL) and water (5 mL) was heated in a steel bomb at 130-140° C. for 3 days. After cooling, the mixture was distributed between water and ethyl acetate, and the organic layer was washed with brine, dried and evaporated. The residue was dissolved in acetone and loaded onto a 4 mm dry silica plate for radial chromatography. The plate was eluted with a 1:1 mixture of petroleum ether and ethyl acetate. Appropriate fractions were collected and evaporated to give 125 mg(12%)of 1-{6-[ethyl-(2-hydroxylethyl)-amino]-2-naphthyl}ethanone.

후처리

  1. temperatureAfter cooling
  2. washthe organic layer was washed with brine
  3. customdried
  4. customevaporated
  5. dissolutionThe residue was dissolved in acetone
  6. washThe plate was eluted with a 1:1 mixture of petroleum ether and ethyl acetate
  7. customAppropriate fractions were collected
  8. customevaporated

출처 및 근거

ORD 기록
ord-ca001cf43e7b4569a0640564d35c01b4
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06660530B2

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