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Ethanol → HCID 136337197, 화합물

HRID 1878025
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HRID 1878025 반응식
[F:1][C:2]1[CH:30]=[CH:29][C:5]([C:6]([NH:8][CH2:9][C:10]2([C:25]([F:28])([F:27])[F:26])[C:15]3[CH:16]=[C:17](C(NC)=O)[CH:18]=[CH:19][C:14]=3[NH:13][C:12](=[O:24])[O:11]2)=[O:7])=[CH:4][CH:3]=1.C1N=CN([C:36]([N:38]2[CH:42]=[N:41]C=C2)=[O:37])C=1.C([OH:45])C>NO.C(OCC)(=O)C>[F:1][C:2]1[CH:30]=[CH:29][C:5]([C:6]([NH:8][CH2:9][C:10]2([C:25]([F:27])([F:28])[F:26])[C:15]3[CH:16]=[C:17]([C:42]4[NH:38][C:36](=[O:45])[O:37][N:41]=4)[CH:18]=[CH:19][C:14]=3[NH:13][C:12](=[O:24])[O:11]2)=[O:7])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 702EthanolHCID 682631,1'-CarbonyldiimidazoleHCID 68490661HCID 68490661, 화합물

생성물 1

HCID 136337197HCID 136337197, 화합물

시약·촉매·용매 2

HCID 787Hydroxylamine용매HCID 8857Ethyl Acetate용매2회

실험 절차

To a solution of N-{[6-cyano-2-oxo-4-(trifluoromethyl)-1,4-dihydro-2H-3,1-benzoxazin-4-yl]methyl}-4-fluorobenzamide (50 mg, 0.127 mmol) synthesized in Example 159 in ethanol (0.5 mL), hydroxylamine (50% aqueous solution, 40 μL) was added, and the solution was stirred overnight at room temperature. The solution was diluted with ethyl acetate, which was washed sequentially with water and saturated brine and then dried over magnesium sulfate. The residue was dissolved in dioxane (1 mL), and under stirring the solution at room temperature, CDI (41 mg, 0.25 mmol) was added thereto. After the reaction solution was stirred at 90° C. for 3 hours, the temperature of the solution was brought to room temperature. Then, the solution was diluted with ethyl acetate, which was washed sequentially with water, 1 N hydrochloric acid and saturated brine and then dried over magnesium sulfate. After the drying agent was removed by filtration, the residue was crystallized with ethanol and water, whereby the objective compound (18 mg, 31%) was obtained as a white solid.

후처리

  1. washwas washed sequentially with water and saturated brine
  2. dry with materialdried over magnesium sulfate
  3. dissolutionThe residue was dissolved in dioxane (1 mL)
  4. stirringunder stirring the solution at room temperature
  5. stirringAfter the reaction solution was stirred at 90° C. for 3 hours
  6. customwas brought to room temperature
  7. washwas washed sequentially with water, 1 N hydrochloric acid and saturated brine
  8. dry with materialdried over magnesium sulfate
  9. customAfter the drying agent was removed by filtration
  10. customthe residue was crystallized with ethanol and water, whereby the objective compound (18 mg, 31%)
  11. customwas obtained as a white solid

출처 및 근거

ORD 기록
ord-44b07d08068442acbaebe13e2cd6fbf5
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08314094B2

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