Formamidine acetate → HCID 178420898, 화합물

HRID 1159174

반응식

HRID 1159174 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178420898HCID 178420898, 화합물수율 93.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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)+).

후처리

  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)

출처 및 근거

ORD 기록
ord-0187ccd68ae8458c8f42c19f3058b348
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812047B2

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