Sulfuric Acid → (+/-)-cis-1 2-Dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene

HRID 365412

反応式

HRID 365412 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C@@H:9]2[CH2:14][CH:13]=[CH:12][CH2:11][C@H:10]2[N+:15]([O-:17])=[O:16])=[CH:5][C:4]=1[O:18][CH3:19].[OH-].[K+].S(=O)(=O)(O)O>C(O)C.CN(C)C=O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C@@H:9]2[CH2:14][CH:13]=[CH:12][CH2:11][C@@H:10]2[N+:15]([O-:17])=[O:16])=[CH:5][C:4]=1[O:18][CH3:19]

参加物

6

反応物 3

HCID 1118Sulfuric AcidHCID 14797Potassium HydroxideHCID 53874256(+/-)-trans-1,2-DI methoxy-4-(2-nitrocyclohex-4-enyl)benzene

生成物 1

HCID 15389588(+/-)-cis-1 2-Dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene収率 86%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 6228Dimethylformamide溶媒

実験手順

10.0 g of (+/-)-trans-1,2-dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene and 20.0 g of potassium hydroxide are dissolved in 150 ml of ethanol and 35 ml of dimethylformamide. A solution of 17.5 ml of conc. sulfuric acid in 60 ml of ethanol is then added dropwise such that the internal temperature does not exceed 4° C. After stirring for 1 h, the mixture is added to 1 l of ice-water, the precipitate is filtered off with suction, washed with water and dried and the crude product is recrystallized from ethanol. M.p.: 82.5-84° C.; yield 86% of theory.

後処理

  1. customdoes not exceed 4° C
  2. filtrationthe precipitate is filtered off with suction
  3. washwashed with water
  4. customdried
  5. customthe crude product is recrystallized from ethanol

出典と根拠

ORDレコード
ord-1c6113ef0cba4125a9bbd14978fd1cc8
出典データセット
uspto-grants-2000_10
特許番号
US06127378

関連ノート

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