Hydroquinone → (+/-)-trans-1,2-DI methoxy-4-(2-nitrocyclohex-4-enyl)benzene

HRID 220108

反応式

HRID 220108 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[N+:11]([O-:13])=[O:12])=[CH:5][C:4]=1[O:14][CH3:15].[C:16]1([CH:23]=CC(O)=[CH:19][CH:18]=1)O.C=CC=C>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C@@H:9]2[CH2:19][CH:18]=[CH:16][CH2:23][C@H:10]2[N+:11]([O-:13])=[O:12])=[CH:5][C:4]=1[O:14][CH3:15]

参加物

5

反応物 3

HCID 785HydroquinoneHCID 78451,3-ButadieneHCID 7096881,2-Dimethoxy-4-(2-nitrovinyl)benzene

生成物 1

HCID 53874256(+/-)-trans-1,2-DI methoxy-4-(2-nitrocyclohex-4-enyl)benzene

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
160 °C

実験手順

50.0 g of 3,4-dimethoxy-ω-nitrostyrene (compound J1), and 1.0 g (9.1 mmol) of hydroquinone are suspended in 200 ml of abs. toluene and treated at −70° C. with 55.0 g (1.02 mol) of liquid 1,3-butadiene. The mixture is stirred at 160° C. for 6 days in an autoclave and then cooled. Some of the solvent is removed on a rotary evaporator, and the resulting precipitate is filtered off with suction and recrystallized in ethanol. M.p.: 113.5-115.5° C.

後処理

  1. temperaturecooled
  2. customSome of the solvent is removed on a rotary evaporator
  3. filtrationthe resulting precipitate is filtered off with suction
  4. customrecrystallized in ethanol

出典と根拠

ORDレコード
ord-b017856a109d4402a420d2b2018985e4
出典データセット
uspto-grants-2012_06
特許番号
US08202880B2

関連ノート

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