Sodium Carbonate → HCID 66933697、化合物

HRID 1401260ノート

反応式

HRID 1401260 の反応式
[Cl: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>[Cl: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

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 10176127Pyridinium chlorideHCID 66933637HCID 66933637、化合物

生成物 1

HCID 66933697HCID 66933697、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
180 °C

実験手順

A mixture of compound of example 32 (0.565 g, 1.31 mmol) and pyridine hydrochloride (1.2 g, 10.38 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.

後処理

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

出典と根拠

ORDレコード
ord-d429ec47920948b78f7914112a605379
出典データセット
uspto-grants-2014_12
特許番号
US08906953B2

反応ノート

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