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

HRID 249205

反応式

HRID 249205 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 108689405-Nitro-1,4,4a,9a-tetrahydroanthraquinone収率 94%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

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%.

後処理

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

出典と根拠

ORDレコード
ord-98389420ba7b4482934597b289074689
出典データセット
uspto-grants-1993_05
特許番号
US05213665

関連ノート

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