4-Heptanamine → HCID 49854109, 화합물

HRID 2410612노트

반응식

HRID 2410612 반응식
[CH3:1][CH2:2][CH2:3][CH:4]([NH2:8])[CH2:5][CH2:6][CH3:7].C([O:11][C:12](=O)[C:13]([C:15]1[CH:23]=[CH:22][C:18]2[O:19][CH2:20][O:21][C:17]=2[CH:16]=1)=[O:14])C>C(O)C>[O:19]1[C:18]2[CH:22]=[CH:23][C:15]([C:13](=[O:14])[C:12]([NH:8][CH:4]([CH2:5][CH2:6][CH3:7])[CH2:3][CH2:2][CH3:1])=[O:11])=[CH:16][C:17]=2[O:21][CH2:20]1

참가 물질

4

반응물 2

HCID 386654-HeptanamineHCID 2758872Ethyl (2H-1,3-benzodioxol-5-yl)(oxo)acetate

생성물 1

HCID 49854109HCID 49854109, 화합물수율 29%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

4-Heptylamine (2.5 g, 22 mmol) was added to a stirred solution of benzo[1,3]dioxol-5-yl-oxo-acetic acid ethyl ester (2 g, 9 mmol)) in ethanol (40 ml)) at room temperature. The resulting reaction mixture was heated to reflux for 4 hours. Then ethanol was distilled off and stirring was continued at 110° C. for 2 hours. The reaction mixture was cooled to room temperature and then 50 ml of THF and 100 ml of aqueous HCl solution were added and stirred for 30 minutes. The mixture was extracted twice with DCM (50 ml). The organic layer was washed twice with water (50 ml) and concentrated in vacuum. The crude product was chromatographed on a silica gel column using ethylacetate/heptane (2:3) as eluent to provide the title compound (0.5 g, 29% yield) as red crystals.

후처리

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureto reflux for 4 hours
  4. distillationThen ethanol was distilled off
  5. addition50 ml of THF and 100 ml of aqueous HCl solution were added
  6. stirringstirred for 30 minutes
  7. extractionThe mixture was extracted twice with DCM (50 ml)
  8. washThe organic layer was washed twice with water (50 ml)
  9. concentrationconcentrated in vacuum
  10. customThe crude product was chromatographed on a silica gel column

출처 및 근거

ORD 기록
ord-3b772ad31eec44688842126b8e36e340
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08816102B2

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