Trifluoroacetic acid → HCID 19960963、化合物

HRID 1900231ノート

反応式

HRID 1900231 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 19960963HCID 19960963、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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-(tri-methylsilylmethyl)-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.

後処理

  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

出典と根拠

ORDレコード
ord-5ddab86a852a4e67922bec3495c36c5d
出典データセット
uspto-grants-1996_11
特許番号
US05574161

反応ノート

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