Ceric ammonium nitrate → HCID 18348642, 화합물

HRID 2268527노트

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HRID 2268527 반응식
[CH2:1]([NH:3][C:4](=[O:31])[O:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH:14]1[CH2:22][C:21]2[C:16](=[C:17]([O:29]C)[C:18]([O:27][CH3:28])=[C:19]([O:25][CH3:26])[C:20]=2[O:23]C)[CH2:15]1)[CH3:2].O=[N+]([O-])[O-].[O-][N+](=O)[O-].[O-][N+](=O)[O-].[O-][N+](=O)[O-].[O-][N+](=O)[O-].[O-][N+](=O)[O-].[Ce+4].[NH4+].[NH4+]>C(#N)C.O>[CH2:1]([NH:3][C:4](=[O:31])[O:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH:14]1[CH2:22][C:21]2[C:20](=[O:23])[C:19]([O:25][CH3:26])=[C:18]([O:27][CH3:28])[C:17](=[O:29])[C:16]=2[CH2:15]1)[CH3:2]

참가 물질

5

반응물 2

HCID 180504Ceric ammonium nitrateHCID 183486018-(4,5,6,7-Tetramethoxyindan-2-yl)octyl N-ethylcarbamate

생성물 1

HCID 18348642HCID 18348642, 화합물수율 55.4%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6342Acetonitrile용매

실험 절차

To a solution of 8-(4,5,6,7-tetramethoxyindan-2-yl)octyl N-ethylcarbamate (1.22 g) in acetonitrile (12 ml) was dropwise added a solution of CAN (3.83 g) in water (12 ml) with cooling with ice. After the reaction mixture was stirred for 15 min, water was added to the reaction mixture, which 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 (hexane to hexane:ethyl acetate=4:1) and then with recrystallization from hexane-ethyl acetate to yield the entitled compound (630 mg) as crystals.

후처리

  1. temperaturewith cooling with ice
  2. extractionwas 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 (hexane to hexane:ethyl acetate=4:1)
  7. customwith recrystallization from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-e1560d0b65da4d92b7c6b65f13e37363
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06326369B1

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