1,3-Butadiene → 5-Nitro-1,4,4a,9a-tetrahydroanthraquinone

HRID 249205

반응식

HRID 249205 반응식
[N+:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]2[C:5]=1[C:6](=[O:15])[CH:7]=[CH:8][C:9]2=[O:14])([O-:3])=[O:2].[CH2:16]=[CH:17][CH:18]=[CH2:19].COCCO>O>[N+:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]2[C:5]=1[C:6](=[O:15])[CH:7]1[CH:8]([C:9]2=[O:14])[CH2:19][CH:18]=[CH:17][CH2:16]1)([O-:3])=[O:2]

참가 물질

5

반응물 3

HCID 78451,3-ButadieneHCID 80192-MethoxyethanolHCID 123364025-Nitronaphthalene-1,4-dione

생성물 1

HCID 108689405-Nitro-1,4,4a,9a-tetrahydroanthraquinone수율 94%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
25 °C

실험 절차

A mixture comprising 10 g of the obtained 5-nitro-1,4-naphthoquinone, 3.3 g of 1,3-butadiene and 40 ml of ethylene glycol monomethyl ether was retained in a 100-milliliter autoclave at 50° C. for 6 hours with stirring. The reaction pressure was initially 1.2 atmospheres and 1.0 atmosphere when the reaction was over. Thereafter, 60 ml of water was added to the reaction mixture and cooled to 25° C. The precipitated crystals were filtered, washed with 30 ml of methyl alcohol and dried under reduced pressure to obtain 11.9 g of white 5-nitro-1,4,4a,9a-tetrahydroanthraquinone having a purity of 98%.

후처리

  1. customThe reaction pressure
  2. filtrationThe precipitated crystals were filtered
  3. washwashed with 30 ml of methyl alcohol
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-98389420ba7b4482934597b289074689
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05213665

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