Acetic Acid → HCID 383402, 화합물

HRID 582205노트

반응식

HRID 582205 반응식
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH2:8][C:9]2=[O:12])=[CH:5][CH:4]=1.[CH:13](=O)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.N1CCCCC1.C(O)(=O)C>C1(C)C=CC=CC=1>[CH:13](=[C:8]1[CH2:7][C:6]2[C:10](=[CH:11][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[C:9]1=[O:12])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 240BenzaldehydeHCID 8082PiperidineHCID 3340366-Methoxy-1-Indanone

생성물 1

HCID 383402HCID 383402, 화합물수율 80%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

6-Methoxy-1-indanone (10 g, 61.2 mmol), benzaldehyde (7.85 g, 74.0 mmol), piperidine (1.05 g, 12.3 mmol), and acetic acid (4.4 g, 74.0 mmol) were refluxed in toluene (150 ml) for 3 hours. After the reaction mixture was cooled to room temperature, the solvent was distilled off under reduced pressure. The residue was diluted with water and extracted with ethyl acetate. The extract was washed serially with saturated saline and water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The resulting crystals were washed with diethyl ether to provide the title compound (yield 2.3 g, 80%).

후처리

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionThe residue was diluted with water
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed serially with saturated saline and water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. washThe resulting crystals were washed with diethyl ether

출처 및 근거

ORD 기록
ord-fb4a4ebe2d8b48d2ba59809d6c3dadbe
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922771

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