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

HRID 357023노트

반응식

HRID 357023 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-5d1e24aefc384d8ba4fafb17322cbc64
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840732

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