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Potassium Carbonate → HCID 86705063, 화합물

HRID 1427308
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HRID 1427308 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([N:14]2[C:22]3[C:17](=[C:18]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[CH:19]=[CH:20][CH:21]=3)[CH:16]=[CH:15]2)([CH2:12][CH3:13])[C:9](=O)[CH3:10])=[CH:4][CH:3]=1.Cl.[NH2:29][OH:30].C([O-])([O-])=O.[K+].[K+]>CCO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([N:14]2[C:22]3[C:17](=[C:18]([NH:23][S:24]([CH3:27])(=[O:26])=[O:25])[CH:19]=[CH:20][CH:21]=3)[CH:16]=[CH:15]2)([CH2:12][CH3:13])[C:9](=[N:29][OH:30])[CH3:10])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 70560671HCID 70560671, 화합물

생성물 1

HCID 86705063HCID 86705063, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
130 °C

실험 절차

To a solution of N-(1-(3-(4-chlorophenyl)-2-oxopentan-3-yl)-1H-indol-4-yl)methanesulfonamide (200 mg, 0.49 mmol), as described in Example 23 Step A, in EtOH (5 mL) was added hydroxylamine hydrochloride (68 mg, 0.99 mmol) and K2CO3 (137 mg, 0.99 mmol). The mixture was stirred at 130° C. under microwave for 2 h. After removing the solvent, the residue was dissolved in ethyl acetate (30 mL). The organic layer was washed with saturated sodium bicarbonate solution (10 mL) and brine (10 mL), dried over sodium sulfate, and then filtered. After removing the organic solvent, the residue was purified by silica gel chromatography eluting with PE/EA (10/1 to 5/1, v/v) to afford the title compound as a white solid. LC/MS m/z=441.9 [M+Na]+.

후처리

  1. customAfter removing the solvent
  2. dissolutionthe residue was dissolved in ethyl acetate (30 mL)
  3. washThe organic layer was washed with saturated sodium bicarbonate solution (10 mL) and brine (10 mL)
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customAfter removing the organic solvent
  7. customthe residue was purified by silica gel chromatography
  8. washeluting with PE/EA (10/1 to 5/1

출처 및 근거

ORD 기록
ord-b4a1497a37cd4ff0b0daebe2d5d53d14
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933113B2

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