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Hydrochloric Acid → 4(1H)-Pyrimidinone, 2-(((2-(dimethylamino)phenyl)methyl)thio)-6-methyl-

HRID 2247849
ノート
印刷プレビュー

反応式

HRID 2247849 の反応式
[CH3:1][C:2]1[NH:7][C:6](=[S:8])[NH:5][C:4](=[O:9])[CH:3]=1.[CH3:10][N:11]([CH3:20])[C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[CH2:14]O.Cl.[OH-].[Na+]>>[CH3:10][N:11]([CH3:20])[C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[CH2:14][S:8][C:6]1[NH:5][C:4](=[O:9])[CH:3]=[C:2]([CH3:1])[N:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 138325Benzenemethanol, 2-(dimethylamino)-HCID 667493Methylthiouracil

生成物 1

HCID 1357442584(1H)-Pyrimidinone, 2-(((2-(dimethylamino)phenyl)methyl)thio)-6-methyl-収率 43%

反応条件

温度
60 °C

実験手順

A mixture containing 0.71 g (5 mmol) of 6-methyl-2-thiouracil, 0.76 g (5 mmol) of 2-dimethylaminobenzyl alcohol (J. Chem. Soc. 1954, 4127) and 5 ml of concentrated hydrochloric acid is stirred at 60° C. for 3 hours, then cooled and made alkaline by adding 5N sodium hydroxide solution under cooling by ice. The mixture is extracted 3 times with 20 ml of chloroform each. After combining the organic phase is washed with sodium carbonate solution and then with saturated sodium chloride solution, dried over anhydrous magnesium sulfate and evaporated. The residue is twice recrystallized from ethyl acetate to yield 0.59 g (43%) of the title compound, m.p.: 151°-153° C.

後処理

  1. temperaturecooled
  2. temperatureunder cooling by ice
  3. extractionThe mixture is extracted 3 times with 20 ml of chloroform each
  4. washis washed with sodium carbonate solution
  5. dry with materialwith saturated sodium chloride solution, dried over anhydrous magnesium sulfate
  6. customevaporated
  7. customThe residue is twice recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-30f7759752ab486692ab855de71aef7d
出典データセット
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05037830

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート