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Trifluoroacetic acid → 5-Methyl-1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazol-7-ol

HRID 585447
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HRID 585447 반응식
[CH3:1][C:2]1[CH:3]=[C:4]2[C:12]3=[C:13]([O:15][CH2:16][CH:17]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[N:11]3[C:10]3[CH2:9][CH2:8][CH2:7][C:6](=[O:24])[C:5]2=3)[CH:14]=1.FC(F)(F)C(O)=O.[Br-].[Li+].C(=O)([O-])[O-].[Li+].[Li+]>C(OCC)(=O)C.C(#N)C.C(Cl)Cl>[CH3:1][C:2]1[CH:3]=[C:4]2[C:12]3=[C:13]([O:15][CH2:16][CH:17]([C:18]4[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=4)[N:11]3[C:10]3[C:5]2=[C:6]([OH:24])[CH:7]=[CH:8][CH:9]=3)[CH:14]=1
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참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 11125Lithium CarbonateHCID 82050Lithium BromideHCID 121486325-methyl-1-phenyl-1,2,9,10-tetrahydro[1,4]oxazino[2,3,4-jk]carbazol-7(8H)-one

생성물 1

HCID 121486335-Methyl-1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazol-7-ol수율 14.5%

시약·촉매·용매 2

HCID 6344
Dichloromethane
용매
HCID 21930812Acetonitrile ethyl acetate용매

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온도
90 °C

실험 절차

To 5-methyl-1-phenyl-1,2,9,10-tetrahydro[1,4]oxazino[2,3,4-jk]carbazol-7(8H)-one (9.0 g, 28.4 mmol) in ethyl acetate/acetonitrile (150 mL/50 mL) is added trifluoroacetic acid (4 mL) and anhydrous cupric chloride (9.7 g, 56.7 mmol). The mixture is heated to reflux at 90° C. for 7 h. The mixture is poured into methylene chloride (500 mL) and filtered to remove inorganic solids. The filtrates are washed with saturated potassium carbonate solution followed by water, dried over magnesium sulfate and concentrated. The residue is dissolved in DMF (20 mL) to which is added lithium bromide (4.2 g, 56.7 mmol) and lithium carbonate (4.9 g, 56.7 mmol). The mixture is heated at 119° C. for 5 h, then partitioned between water and CH2Cl2. The organic layer is washed twice with brine (30 mL). Column chromatography (200 g silica gel) using EtOAc/hexanes (20/80) as eluent gave 1.3 g (14.5%) of 5-methyl-1-phenyl-1,2-dihydro[1,4]oxazino[2,3,4-jk]carbazol-7-ol.

후처리

  1. temperatureThe mixture is heated
  2. filtrationfiltered
  3. customto remove inorganic solids
  4. washThe filtrates are washed with saturated potassium carbonate solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. dissolutionThe residue is dissolved in DMF (20 mL) to which
  8. temperatureThe mixture is heated at 119° C. for 5 h
  9. custompartitioned between water and CH2Cl2
  10. washThe organic layer is washed twice with brine (30 mL)

출처 및 근거

ORD 기록
ord-463b320f63b74f0b858f34c5f4dd4a14
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06932961B1

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