Trifluoroacetic acid → HCID 19960963, 화합물

HRID 1608681노트

반응식

HRID 1608681 반응식
[C:1]([C:3]1[CH2:4][O:5][CH2:6][CH:7]=1)#[N:2].C(N(CC)CC)C.FC(F)(F)C(O)=O.[CH2:22]([N:29]([CH2:35]OC)[CH2:30][Si](C)(C)C)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>C(Cl)Cl>[CH2:22]([N:29]1[CH2:30][C:3]2([C:1]#[N:2])[CH:7]([CH2:6][O:5][CH2:4]2)[CH2:35]1)[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 8471TriethylamineHCID 353442Benzyl(methoxymethyl)((trimethylsilyl)methyl)amineHCID 199609552,5-Dihydrofuran-3-carbonitrile

생성물 1

HCID 19960963HCID 19960963, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 5.2 g (24.6 mmol, 46% strength) of 3-cyano-2,5-dihydrofuran in 50 ml of absolute methylene chloride is mixed with 0.3 g of triethylamine and 0.3 g of trifluoroacetic acid, the mixture is heated under reflux and then 7 g (29.5 mmol) of N-benzyl-N-methoxymethyl-N-(trimethylsilylmethyl)-amine are added dropwise. Subsequently, the mixture is heated under reflux for 2 hours and the solution is washed with saturated sodium hydrogen carbonate solution, dried over magnesium sulphate, concentrated and distilled.

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux
  3. temperatureSubsequently, the mixture is heated
  4. temperatureunder reflux for 2 hours
  5. washthe solution is washed with saturated sodium hydrogen carbonate solution
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated
  8. distillationdistilled

출처 및 근거

ORD 기록
ord-f11cdc9523fc4d72aaae35bc0dc61dec
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05395944

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