Hydrogen Bromide → 1(2H)-Naphthalenone, 3,4-dihydro-6,7-dihydroxy-

HRID 2188216노트

반응식

HRID 2188216 반응식
C[O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13]C)[C:9](=[O:15])[CH2:8][CH2:7][CH2:6]2.Br>O>[OH:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[OH:13])[C:9](=[O:15])[CH2:8][CH2:7][CH2:6]2

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 2668163,4-Dihydro-6,7-dimethoxy-1(2H)-naphthalenone

생성물 1

HCID 6012071(2H)-Naphthalenone, 3,4-dihydro-6,7-dihydroxy-수율 72.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 6,7-dimethoxy-3,4-dihydro-2H-naphthalene-1-one (15.0 g) and 48% aqueous hydrobromic acid (60 cm3) was heated under reflux for 18 h. Upon cooling to room temperature, water (100 cm3) was added and the resulting aqueous mass was extracted with ethyl acetate (3×100 cm3). The combined extracts were dried (Na2SO4), filtered and evaporated to dryness to leave a brown powder. This was recrystallised from acetonitrile to afford the title compound (9.4 g) as a red powder.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 18 h
  3. extractionthe resulting aqueous mass was extracted with ethyl acetate (3×100 cm3)
  4. dry with materialThe combined extracts were dried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customto leave a brown powder
  8. customThis was recrystallised from acetonitrile

출처 및 근거

ORD 기록
ord-99846a97f2274c68a46c23bba997f718
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06410592B1

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