Sodium Carbonate → HCID 67409414, 화합물

HRID 1401257노트

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HRID 1401257 반응식
[Br:1][C:2]1[C:3]([Cl:31])=[C:4]([C:8]2[O:9][C:10]3[C:15]([C:16](=[O:18])[CH:17]=2)=[C:14]([O:19]C)[CH:13]=[C:12]([O:21]C)[C:11]=3[C@@H:23]2[CH2:27][CH2:26][N:25]([CH3:28])[C@H:24]2[CH2:29][OH:30])[CH:5]=[CH:6][CH:7]=1.Cl.N1C=CC=CC=1.C([O-])([O-])=O.[Na+].[Na+]>CO>[Br:1][C:2]1[C:3]([Cl:31])=[C:4]([C:8]2[O:9][C:10]3[C:15]([C:16](=[O:18])[CH:17]=2)=[C:14]([OH:19])[CH:13]=[C:12]([OH:21])[C:11]=3[C@@H:23]2[CH2:27][CH2:26][N:25]([CH3:28])[C@H:24]2[CH2:29][OH:30])[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 10176127Pyridinium chlorideHCID 67397754HCID 67397754, 화합물

생성물 1

HCID 67409414HCID 67409414, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

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온도
180 °C

실험 절차

A mixture of compound of example 28 (0.280 g, 0.550 mmol) and pyridine hydrochloride (0.780 g, 6.74 mmol) was heated at 180° C. for a period of 2.5 hours. The reaction mixture was diluted with methanol (60 mL) and basified with solid Na2CO3 to pH 10. The reaction mixture was filtered, and washed with methanol. The organic layer was concentrated and the residue purified by column chromatography using 0.01% ammonia and 4.5% methanol in chloroform as eluent to afford the title compound.

후처리

  1. filtrationThe reaction mixture was filtered
  2. washwashed with methanol
  3. concentrationThe organic layer was concentrated
  4. customthe residue purified by column chromatography

출처 및 근거

ORD 기록
ord-30abeabd2efd4c519eccf3481ba0294c
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08906953B2

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