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Sodium Hydroxide → HCID 66633913, 화합물

HRID 1961464
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HRID 1961464 반응식
[CH3:1][C:2]1[NH:3][C:4]2[C:9]([C:10](=O)[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:8][CH:7]=[CH:6][N:5]=2.[OH-].[Na+].O=P(Cl)(Cl)[Cl:22]>>[Cl:22][C:10]1[C:9]2[C:4](=[N:5][CH:6]=[CH:7][CH:8]=2)[N:3]=[C:2]([CH3:1])[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13]
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참가 물질

4

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 11085642HCID 11085642, 화합물

생성물 1

HCID 66633913HCID 66633913, 화합물수율 95%

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온도
100 °C

실험 절차

Ethyl 2-methyl-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate (5.18 mg, 2.23 mmol) was dissolved in POCl3. The mixture was heated to 100° C. for 1.0 h. The mixture was allowed to cool and then it was carefully poured into ice-water (250 ml). The mixture was neutralized with solid NaOH. The product was extracted with EtOAc. The combined organic extracts were dried (MgSO4), filtered and concentrated. Purification was done by flash chromatography (CH2Cl2/MeOH 97:3→96:4) giving 531 mg (95%) of the title compound.

후처리

  1. temperatureto cool
  2. extractionThe product was extracted with EtOAc
  3. dry with materialThe combined organic extracts were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification

출처 및 근거

ORD 기록
ord-44f2770df1e24de0a080e4ce4de6f923
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08415333B2

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