Acetic Acid → Ethyl 3-(methylamino)-3-phenylacrylate

HRID 1879269노트

반응식

HRID 1879269 반응식
[C:1]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:15][NH2:16].C(O)(=O)C>CCO>[CH3:15][NH:16][C:1]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[CH:9][C:10]([O:12][CH2:13][CH3:14])=[O:11]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 6329MethylamineHCID 7170Ethyl benzoylacetate

생성물 1

HCID 58005139Ethyl 3-(methylamino)-3-phenylacrylate수율 20%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of ethyl benzoylacetate and methylamine (2M in THF, 8 eq.) in EtOH (1 M) was added acetic acid (8 eq.). The reaction mixture was heated to reflux and stirred for three days. The reaction mixture was concentrated and partition between DCM and 1N HCl. The layers were separated and the organic layer was dried (Na2SO4), filtered and concentrated to give the title compound 112 (20%) which was used with no further purification.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux
  3. concentrationThe reaction mixture was concentrated
  4. custompartition between DCM and 1N HCl
  5. customThe layers were separated
  6. dry with materialthe organic layer was dried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-dc5ed1a494244fd988252b8f61b6b4d3
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314062B2

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