Sodium Carbonate → HCID 68644254、化合物

HRID 1158782ノート

反応式

HRID 1158782 の反応式
C([O:8][C:9]1[CH:10]=[C:11]([CH:15]([OH:38])[CH2:16][N:17]([CH2:35][CH2:36]O)[C:18]([C:20]2[C:21]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[N:22][C:23]([N:26]([CH3:28])[CH3:27])=[N:24][CH:25]=2)=[O:19])[CH:12]=[CH:13][CH:14]=1)C1C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>>[CH3:27][N:26]([CH3:28])[C:23]1[N:22]=[C:21]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:20]([C:18]([N:17]2[CH2:35][CH2:36][O:38][CH:15]([C:11]3[CH:12]=[CH:13][CH:14]=[C:9]([OH:8])[CH:10]=3)[CH2:16]2)=[O:19])=[CH:25][N:24]=1

参加物

3

反応物 2

HCID 10340Sodium CarbonateHCID 86610923HCID 86610923、化合物

生成物 1

HCID 68644254HCID 68644254、化合物収率 14.6%

反応条件

温度
100 °C

実験手順

To 2-dimethylamino-4-phenylpyrimidin-5-carboxylic acid [2-(3-benzyloxyphenyl)-2-hydroxyethyl]-(2-hydroxyethyl)amide (0.20 g, 0.39 mmol) 48% hydrogen bromide solution (4 ml) is added. The mixture is heated at 100° C. for 1 hour, cooled to room temperature, poured onto water and neutralized (pH 7) with sodium carbonate solution. The precipitate is filtered oft washed with water and dried. The crude product is chromatographed on silicagel using chloroform and chloroform-ethyl acetate 9:1 mixture as eluent. 0.023 g light-yellow title compound is obtained, m.p.: 140° C.

後処理

  1. temperaturecooled to room temperature
  2. filtrationThe precipitate is filtered oft
  3. washwashed with water
  4. customdried
  5. customThe crude product is chromatographed on silicagel

出典と根拠

ORDレコード
ord-d3badd827fa54996a8cd8fced8c8559d
出典データセット
uspto-grants-2010_10
特許番号
US07812031B2

反応ノート

読み込み中…