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Potassium Carbonate → HCID 68785003, 화합물

HRID 2266490
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HRID 2266490 반응식
[CH3:1][O:2][C:3](=[O:27])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]2[C:7]=1[C:8]([CH3:26])=[C:9]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)[C:10](=[O:17])[NH:11]2.C(=O)([O-])[O-].[K+].[K+].Cl[C:35](OC(=O)C)([F:37])[F:36]>O>[CH3:1][O:2][C:3](=[O:27])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]2[C:7]=1[C:8]([CH3:26])=[C:9]([CH2:18][C:19]1[CH:20]=[CH:21][C:22]([Cl:25])=[CH:23][CH:24]=1)[C:10]([O:17][CH:35]([F:37])[F:36])=[N:11]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 68608867HCID 68608867, 화합물HCID 86613376Chlorodifluoromethyl acetate

생성물 1

HCID 68785003HCID 68785003, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
70 °C

실험 절차

A mixture of [3-(4-chlorobenzyl)-8-fluoro-4-methyl-2-oxo-1,2-dihydroquinolin-5-yloxy]acetic acid methyl ester (1.0 g), N7N-dimethylformamide (15 mL), potassium carbonate (0.89 g) and acetic acid chlorodifluoromethyl ester (1.1 mL) was stirred at 70° C. for 18 hours. The mixture was diluted with water, extracted with ethyl acetate and the combined extracts dried over magnesium sulfate. The solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel, eluting with a mixture of pentane and dichloromethane (4:1 by volume) gave title compound as a white solid, 0.49 g.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialthe combined extracts dried over magnesium sulfate
  3. customThe solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel
  4. washeluting with a mixture of pentane and dichloromethane (4:1 by volume)

출처 및 근거

ORD 기록
ord-21f02fb816e843bc816e365e6f1bad68
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858640B2

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