Sodium Carbonate → HCID 68644254, 화합물

HRID 1158782노트

반응식

HRID 1158782 반응식
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

참가 물질

3

반응물 2

HCID 10340Sodium CarbonateHCID 86610923HCID 86610923, 화합물

생성물 1

HCID 68644254HCID 68644254, 화합물수율 14.6%

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d3badd827fa54996a8cd8fced8c8559d
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812031B2

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