1-Iodo-4-nitrobenzene → p-(1-Trifluoromethylheptyloxy)nitrobenzene

HRID 372931

反応式

HRID 372931 の反応式
[H-].[Na+].[F:3][C:4]([F:14])([F:13])[CH:5]([OH:12])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[H][H].[Na].I[C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1>O.CN(C=O)C>[F:3][C:4]([F:13])([F:14])[CH:5]([O:12][C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]

参加物

8

反応物 5

HCID 124951-Iodo-4-nitrobenzeneHCID 24758Sodium hydrideHCID 978042-Octanol, 1,1,1-trifluoro-2 回HCID 5360545SodiumHCID 178418361HCID 178418361、化合物

生成物 1

HCID 15123947p-(1-Trifluoromethylheptyloxy)nitrobenzene

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Into 200 ml of dry DMF containing 2.0 g of sodium hydride (purity 60%), were added dropwise 9.2 g of S-form oa 1-trifluoromethyl-heptanol, at room temperature with such a speed not causing too rapid generation of hydrogen, to prepare sodium salt (alkoxide) of S-form oa 1-trifluoromethyl-heptanol. After the addition was over, stirring was continued further an hour at room temperature, followed by adding thereto 12.4 g of p-iodo-nitro-benzene and then refluxing for 2 hours. After cooling, the product was introduced into iced water, and extracted with hexane. The hexane phase was washed subsequently with water, 1N-hydrochloric acid aqueous solution and then water, followed by purifying with silica gell column to obtain 7.7 g of oily oa p-(1-trifluoromethylheptyloxy)- nitrobenzene.

後処理

  1. customat room temperature
  2. additionAfter the addition
  3. waitwas continued further an hour at room temperature
  4. additionby adding
  5. temperatureAfter cooling
  6. extractionextracted with hexane
  7. washThe hexane phase was washed subsequently with water, 1N-hydrochloric acid aqueous solution
  8. customby purifying with silica gell column

出典と根拠

ORDレコード
ord-cf72626921c74d82b46ed2443b5116fd
出典データセット
uspto-grants-1992_11
特許番号
US05160662

関連ノート

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