Sodium hydride → p-(1-Trifluoromethyl-heptyloxy)-benzonitrile

HRID 372929

반응식

HRID 372929 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:26]=[CH:25][C:22]([C:23]#[N:24])=[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:26]=[CH:25][C:22]([C:23]#[N:24])=[CH:21][CH:20]=1)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]

참가 물질

8

반응물 5

HCID 24758Sodium hydrideHCID 764674-IodobenzonitrileHCID 978042-Octanol, 1,1,1-trifluoro-2회HCID 5360545SodiumHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 15724839p-(1-Trifluoromethyl-heptyloxy)-benzonitrile

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

Into 100 ml of dry DMF containing 0.86 g of sodium hydride (purity 60%), were added dropwise 3.9 g of R-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 R-form oa 1-trifluoromethyl-heptanol. After addition was over, stirring was continued further an hour at room temperature, followed by adding thereto 4.80 g of p-iodo-benzonitrile 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-HCl aqueous solution and then water, followed by purifying with silica gel column to obtain 5.16 g of oily oa p-(1-trifluoromethyl-heptyloxy)- benzonitrile.

후처리

  1. customat room temperature
  2. additionAfter 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-HCl aqueous solution
  8. customby purifying with silica gel column

출처 및 근거

ORD 기록
ord-2b8b5b7465ef4adc9b1eda4352119f95
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05160662

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