Sulfuric acid magnesium salt (1:1) → 4-Amino-2-(4-hydroxybutylthio)pyrimidine

HRID 357023ノート

反応式

HRID 357023 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([S:8][CH2:9][CH2:10][CH2:11][C:12](OCC)=[O:13])[N:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[Al].S([O-])([O-])(=O)=O.[Mg+2]>O1CCCC1.O>[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([S:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13])[N:3]=1

参加物

7

反応物 4

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 5359268AluminumHCID 189367844-Amino-2-(3-ethoxycarbonylpropylthio)pyrimidineHCID 21226445Aluminium lithium hydride

生成物 1

HCID 189368114-Amino-2-(4-hydroxybutylthio)pyrimidine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

To a solution of 6.03 g (25 mmol) of 4-amino-2-(3-ethoxycarbonylpropylthio)pyrimidine in 150 ml of tetrahydrofuran, 0.949 g (150 mmol) of lithium aluminum hydride was added at room temperature, followed by stirring at 60° C. for 2 hours. After the reaction mixture was cooled, water was added little by little to decompose the excess aluminum reagent. After anhydrous magnesium sulfate was added to the mixture, the precipitate was filtered off, after which the solvent was distilled off to yield 8.85 g (88.8%, white crystal) of the desired product.

後処理

  1. temperatureAfter the reaction mixture was cooled
  2. filtrationthe precipitate was filtered off
  3. distillationafter which the solvent was distilled off

出典と根拠

ORDレコード
ord-5d1e24aefc384d8ba4fafb17322cbc64
出典データセット
uspto-grants-1998_11
特許番号
US05840732

反応ノート

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