Sodium hydride → 2-n-Butyl-3-n-propyl-3H-thieno[2,3-d]pyrimidin-4-one

HRID 650933노트

반응식

HRID 650933 반응식
[H-].[Na+].[CH2:3]([NH:6][C:7]([C:9]1[CH:13]=[CH:12][S:11][C:10]=1[N:14]=[C:15]([CH2:18][CH2:19][CH2:20][CH3:21])OC)=[O:8])[CH2:4][CH3:5]>C1COCC1>[CH2:18]([C:15]1[N:6]([CH2:3][CH2:4][CH3:5])[C:7](=[O:8])[C:9]2[CH:13]=[CH:12][S:11][C:10]=2[N:14]=1)[CH2:19][CH2:20][CH3:21]

참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 539289552-(1-n-Butyl-1-methoxymethyleneamino)-thiophene-3-carboxylicacid propylamide

생성물 1

HCID 217104152-n-Butyl-3-n-propyl-3H-thieno[2,3-d]pyrimidin-4-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In a sulfonation flask, 0.85 g of 2-(1-n-butyl-1-methoxymethyleneamino)-thiophene-3-carboxylicacid propylamide is dissolved in 20 ml of absolute THF and 0.15 g of a ca. 55% NaH dispersion is added in small portions. The mixture is stirred for 15 minutes at room temperature and 1 hour at reflux temperature. Then the solvent is removed in a water jet vacuum and the residue taken up in ethylacetate. The organic phase is washed twice with water and after drying of the organic phase with sodium sulfate, the solvent is removed in a water jet vacuum. The resulting crude product (yleld: 0.8 g of 2-n-butyl-3-n-propyl-3H-thieno[2,3-d]-pyrimidine-4-one in the form of a brown liquid) can be used without further purification for the halogenation step.

후처리

  1. temperatureat reflux temperature
  2. customThen the solvent is removed in a water jet vacuum
  3. washThe organic phase is washed twice with water
  4. dry with materialafter drying of the organic phase with sodium sulfate
  5. customthe solvent is removed in a water jet vacuum
  6. customThe resulting crude product (yleld: 0.8 g of 2-n-butyl-3-n-propyl-3H-thieno[2,3-d]-pyrimidine-4-one in the form of a brown liquid) can be used without further purification for the halogenation step

출처 및 근거

ORD 기록
ord-a8d2352cfd75413d8ba312d5a592427b
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06277858B1

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