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Sodium Carbonate → HCID 67408796, 화합물

HRID 1401278
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HRID 1401278 반응식
[I:1][C:2]1[CH:3]=[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>[I:1][C:2]1[CH:3]=[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
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참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 10176127Pyridinium chlorideHCID 67409286HCID 67409286, 화합물

생성물 1

HCID 67408796HCID 67408796, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

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온도
180 °C

실험 절차

A mixture of compound of example 68 (0.4 g, 0.70 mmol) and pyridine hydrochloride (0.327 g, 2.83 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-3c5cfb62e3ab4284b2bb05a3d3b1e312
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08906953B2

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