Nitromethane → HCID 58718575, 화합물

HRID 897173노트

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HRID 897173 반응식
[CH2:1]([O:3][C:4](=[O:13])[CH:5]=[C:6]1[CH2:10][C@@H:9]([CH3:11])[C@H:8]([CH3:12])[CH2:7]1)[CH3:2].CCCC[N+](CCCC)(CCCC)CCCC.[F-].[N+:32]([CH3:35])([O-:34])=[O:33]>C1COCC1.C(OCC)(=O)C>[CH2:1]([O:3][C:4](=[O:13])[CH2:5][C:6]1([CH2:35][N+:32]([O-:34])=[O:33])[CH2:7][C@@H:8]([CH3:12])[C@H:9]([CH3:11])[CH2:10]1)[CH3:2]

참가 물질

6

반응물 3

HCID 6375NitromethaneHCID 2724141Tetrabutylammonium FluorideHCID 58718576HCID 58718576, 화합물

생성물 1

HCID 58718575HCID 58718575, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

To a solution of (2) (4.24 g, 23.3 mmol) in THF (15 mL) was added TBAF (32 mL of a 1 M solution in THF, 32 mmol) followed by nitromethane (3 mL) and the reaction heated at 60° C. for 8 hours. After cooling, the reaction mixture was diluted with ethyl acetate (150 mL) and washed with 2N HCl (40 mL) then saturated brine (50 mL). Column chromatography (10:1 heptane/ethyl acetate) gave the product as an oil, 2.24 g, 40%.

후처리

  1. temperatureAfter cooling
  2. washwashed with 2N HCl (40 mL)

출처 및 근거

ORD 기록
ord-cdfd1f60f02e4468b97cca3585324634
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06921835B2

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