Nitromethane → HCID 11275397, 화합물

HRID 458007노트

반응식

HRID 458007 반응식
[NH:1]1[C:5]([CH2:6][C:7]2(C#N)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)=NN=N1.[N+:15]([CH3:18])([O-:17])=[O:16].[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1.C(OCC)(=O)C>[N+:15]([CH2:18][C:7]1([CH2:6][C:5]#[N:1])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([O-:17])=[O:16]

참가 물질

6

반응물 3

HCID 6375NitromethaneHCID 2724141Tetrabutylammonium FluorideHCID 178509433HCID 178509433, 화합물2회

생성물 1

HCID 11275397HCID 11275397, 화합물수율 71%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

The nitrile (compound 2, 0.78 g, 6.44 mmol), nitromethane (0.80 g, 13.11 mmol) and tetrabutyl ammonium fluoride (1.0 M in tetrahydrofuran, 10 mL, 10 mmol) were heated in 20 mL tetrahydrofuran to 70° C. overnight. The reaction mixture was diluted with ethyl acetate and washed with dilute hydrochloric acid and water, dried over magnesium sulphate, filtered, and evaporated to dryness. The residue was purified by chromatography on silica eluting with heptane/ethyl acetate 3:1 to give the required product as a yellow oil (0.83 g, 71%).

후처리

  1. washwashed with dilute hydrochloric acid and water
  2. dry with materialdried over magnesium sulphate
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customThe residue was purified by chromatography on silica eluting with heptane/ethyl acetate 3:1

출처 및 근거

ORD 기록
ord-93d5e0f6971d4be6ad999c693711a8f2
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189747B2

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