5-Benzyl-5-azaspiro[2.4]heptan-7-one → 5-Benzyl-7-methylene-5-azaspiro[2.4]heptane

HRID 1010803ノート

反応式

HRID 1010803 の反応式
[CH2:1]([N:8]1[CH2:14][C:13](=O)[C:10]2([CH2:12][CH2:11]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[Zn][CH2:18][Zn]C[Zn]Br.C1OCCC1>O1CCCC1>[CH2:1]([N:8]1[CH2:14][C:13](=[CH2:18])[C:10]2([CH2:12][CH2:11]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 103527905-Benzyl-5-azaspiro[2.4]heptan-7-oneHCID 178420636HCID 178420636、化合物

生成物 1

HCID 167351155-Benzyl-7-methylene-5-azaspiro[2.4]heptane

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5-benzyl-5-azaspiro[2.4]heptan-7-one (300 mg) was dissolved into anhydrous tetrahydrofuran (10 ml) and Nysted reagent (1.5 eq, 20% solution) was added to the reaction. The reaction was stirred at RT for two days and quenched with NH4Cl solution and extracted with EtOAc followed by washing with water, then brine and dried over Na2SO4 and purified with silica gel column to give the titled compound. Mass: (M+1), 200

後処理

  1. additionwas added to the reaction
  2. customquenched with NH4Cl solution
  3. extractionextracted with EtOAc
  4. washby washing with water
  5. dry with materialbrine and dried over Na2SO4
  6. custompurified with silica gel column

出典と根拠

ORDレコード
ord-670c83ba180e48f8ab407d800d63c3a5
出典データセット
uspto-grants-2011_07
特許番号
US07977346B2

反応ノート

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