Ceric ammonium nitrate → HCID 21919159, 화합물

HRID 1245201노트

반응식

HRID 1245201 반응식
C[O:2][C:3]1[C:4]([CH3:33])=[C:5]([C:24]([O:31]C)=[C:25]([O:29][CH3:30])[C:26]=1[O:27][CH3:28])[CH2:6][C:7]1[CH:8]=[CH:9][C:10]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=2)=[C:11]([CH:15]=1)[C:12]([OH:14])=[O:13].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>[CH3:28][O:27][C:26]1[C:3](=[O:2])[C:4]([CH3:33])=[C:5]([CH2:6][C:7]2[CH:8]=[CH:9][C:10]([C:16]3[CH:17]=[CH:18][C:19]([O:22][CH3:23])=[CH:20][CH:21]=3)=[C:11]([CH:15]=2)[C:12]([OH:14])=[O:13])[C:24](=[O:31])[C:25]=1[O:29][CH3:30]

참가 물질

5

반응물 2

HCID 180504Ceric ammonium nitrateHCID 121472845-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-(4-methoxyphenyl)benzoic acid

생성물 1

HCID 21919159HCID 21919159, 화합물수율 63%

시약·촉매·용매 2

HCID 962Water용매2회HCID 6342Acetonitrile용매

실험 절차

5-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-(4-methoxy-phenyl)benzoic acid (440 mg, 0.9734 mmol) was dissolved in a mixed solvent of acetonitrile (30 ml) and water (10 ml), then CAN (1.10 g, 2.0072 mmol) was added thereto at room temperature and the mixture was stirred for 3 hour. The reaction solution was poured into water and extracted with ether. The extract was washed with water and dried and the solvent was evaporated therefrom. The residue was purified by silica gel column chromatography (5% methanol-methylene chloride) to give the title compound (259 mg, 0.6137 mmol, 63%).

후처리

  1. extractionextracted with ether
  2. washThe extract was washed with water
  3. customdried
  4. customthe solvent was evaporated
  5. customThe residue was purified by silica gel column chromatography (5% methanol-methylene chloride)

출처 및 근거

ORD 기록
ord-582bf45822c44a6ea99578ed50cfd7d4
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07122543B2

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