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Water → N-[8-(4,5,6,7-Tetramethoxyindan-2-yl)octyl]acetamide

HRID 2268477
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HRID 2268477 반응식
[CH3:1][O:2][C:3]1[C:11]([O:12][CH3:13])=[C:10]([O:14][CH3:15])[C:9]([O:16][CH3:17])=[C:8]2[C:4]=1[CH2:5][CH:6]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH2:26])[CH2:7]2.C(=O)([O-])[O-].[K+].[K+].O.[C:34](Cl)(=[O:36])[CH3:35]>C(OCC)(=O)C>[CH3:17][O:16][C:9]1[C:10]([O:14][CH3:15])=[C:11]([O:12][CH3:13])[C:3]([O:2][CH3:1])=[C:4]2[C:8]=1[CH2:7][CH:6]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH:26][C:34](=[O:36])[CH3:35])[CH2:5]2
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참가 물질

6

반응물 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 11430Potassium CarbonateHCID 183485288-(4,5,6,7-Tetramethoxyindan-2-yl)octylamine

생성물 1

HCID 18348615N-[8-(4,5,6,7-Tetramethoxyindan-2-yl)octyl]acetamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a mixture of 8-(4,5,6,7-tetramethoxyindan-2-yl)octylamine (878 mg), potassiumcarbonate (2.54 g),water (16 ml), and ethyl acetate (16 ml) was dropwise added acetyl chloride (0.341 ml) with cooling with ice. After being stirred for 15 min, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo. The residue was purified by silica gel column chromatography (ethyl acetate) and then with recrystallization (hexane-ethyl acetate) to give the entitled compound (0.830 g) as crystals.

후처리

  1. temperaturewith cooling with ice
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated aqueous sodium chloride
  4. customdried
  5. customThe solvent was removed in vacuo
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate)
  7. customwith recrystallization (hexane-ethyl acetate)

출처 및 근거

ORD 기록
ord-3f2a4129b7954ec48d69da6ee93dffdc
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06326369B1

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