Dimethylformamide → HCID 22459155, 화합물

HRID 2185030노트

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HRID 2185030 반응식
FC1(C2C=CC=C([O:15][CH2:16][CH2:17][CH2:18][O:19][C:20]3[CH:25]=[CH:24][C:23]([O:26][C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)=[CH:22][C:21]=3[CH2:33][CH2:34][CH3:35])C=2)SC(=O)NC1=O.O([C:43]1[CH:48]=[CH:47][C:46](O)=[C:45]([CH2:50][CH2:51]C)[CH:44]=1)C1C=CC=CC=1.[C:53](=O)([O-])[O-:54].[Cs+].[Cs+].CN(C=[O:63])C>>[CH2:33]([C:21]1[CH:22]=[C:23]([O:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:24]=[CH:25][C:20]=1[O:19][CH2:18][CH2:17][CH2:16][O:15][C:48]1[CH:43]=[CH:44][C:45]([CH2:50][C:51]([O:54][CH3:53])=[O:63])=[CH:46][CH:47]=1)[CH2:34][CH3:35]

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 9848632HCID 9848632, 화합물HCID 154629044-Phenoxy-2-propylphenol

생성물 1

HCID 22459155HCID 22459155, 화합물

실험 절차

A solution of the product from Step A (11.0 g, 38.58 mmol), 4-phenoxy-2-propylphenol (PCT Application WO97/28115; 8.0 g, 35.07 mmol) and cesium carbonate (12.0 g, 36.82 mmol) in DMF (80 mL) was stirred at 40° C. overnight. The reaction mixture was partitioned between ethyl acetate and 0.2N HCl. The organic layer was washed twice with water, then dried over sodium sulfate. The organic layer was filtered and evaporated to an oil which was chromatographed over silica gel with 10% of ethyl acetate in hexane to afford the title compound.

후처리

  1. customThe reaction mixture was partitioned between ethyl acetate and 0.2N HCl
  2. washThe organic layer was washed twice with water
  3. dry with materialdried over sodium sulfate
  4. filtrationThe organic layer was filtered
  5. customevaporated to an oil which
  6. customwas chromatographed over silica gel with 10% of ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-bdc8da64ba1745abb1a7d2c80f586e1b
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06399640B1

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