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

HRID 372931

반응식

HRID 372931 반응식
[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]

참가 물질

8

반응물 5

HCID 124951-Iodo-4-nitrobenzeneHCID 24758Sodium hydrideHCID 978042-Octanol, 1,1,1-trifluoro-2회HCID 5360545SodiumHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 15123947p-(1-Trifluoromethylheptyloxy)nitrobenzene

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cf72626921c74d82b46ed2443b5116fd
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05160662

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