Formamidine acetate → HCID 178420898、化合物

HRID 1159174ノート

反応式

HRID 1159174 の反応式
[C:1]1([CH2:7][C@@H:8]([NH2:11])[CH2:9][NH2:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:12](O)(=O)C.C(N)=N>C(O)C>[CH2:7]([C@@H:8]1[CH2:9][NH:10][CH:12]=[N:11]1)[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 160693Formamidine acetateHCID 12699299(2R)-3-Phenylpropane-1,2-diamine

生成物 1

HCID 178420898HCID 178420898、化合物収率 93.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of (2R)-3-phenyl-1,2-propanediamine (0.20 g, 1.33 mmol) in ethanol (5 ml) was added formamidine acetate (0.15 g, 1.45 mmol) and the mixture was stirred overnight at room temperature. The solvent was evaporated, sodium hydroxide (2N, 5 ml) was added and the mixture was extracted 3 times with dichloromethane (10 ml). The combined organic layers were dried over magnesium sulfate and evaporated. The residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10) to yield a colorless oil (0.20 g, 92%); MS (ISP): 161.4 ((M+H)+).

後処理

  1. customThe solvent was evaporated
  2. additionsodium hydroxide (2N, 5 ml) was added
  3. extractionthe mixture was extracted 3 times with dichloromethane (10 ml)
  4. dry with materialThe combined organic layers were dried over magnesium sulfate
  5. customevaporated
  6. customThe residue was purified by chromatography (column: Isolute® Flash-NH2 from Separtis; eluent:ethyl acetate/methanol=90:10)

出典と根拠

ORDレコード
ord-0187ccd68ae8458c8f42c19f3058b348
出典データセット
uspto-grants-2010_10
特許番号
US07812047B2

反応ノート

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