Sodium → HCID 11357207, 화합물

HRID 1384858노트

반응식

HRID 1384858 반응식
[Na].CS[C:4]1[N:5]([CH2:14][CH2:15][CH3:16])[C:6](=[O:13])[C:7]2[CH:12]=[CH:11][S:10][C:8]=2[N:9]=1>C(O)CC>[CH2:6]([O:13][C:4]1[N:5]([CH2:14][CH2:15][CH3:16])[C:6](=[O:13])[C:7]2[CH:12]=[CH:11][S:10][C:8]=2[N:9]=1)[CH2:7][CH3:8]

참가 물질

4

반응물 2

HCID 5360545SodiumHCID 18434022HCID 18434022, 화합물

생성물 1

HCID 11357207HCID 11357207, 화합물수율 106.2%

시약·촉매·용매 1

HCID 10311-Propanol용매

실험 절차

In a sulfonation flask, 12.5 g (0.15 mol) of sodium propylate and 12.0 g (0.05 mol) 2-methylsulfanyl-3-propyl-3H-thieno[2.3-d]pyrimidin-4-one are stirred in 120 ml of absolute n-propanol for 4 hours under nitrogen at reflux temperature. The n-propanol is then removed in a water-jet vacuum and the residue taken up in ethyl acetate/water and the organic phase is extracted twice with water. The organic phase is dried over sodium sulfate and the solvent removed in the water-jet vacuum, giving the crude product, which is then purified by column chromatography over silica gel (eluant: ethyl acetate/hexane=1:3). 6.7 g of 2-propoxy-3-propyl-3H-thieno[2.3-d]pyrimidin-4-one are obtained in the form of a brown resin (1H-NMR-data see table 1 1).

후처리

  1. temperatureat reflux temperature
  2. customThe n-propanol is then removed in a water-jet vacuum
  3. extractionthe organic phase is extracted twice with water
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customthe solvent removed in the water-jet vacuum
  6. customgiving the crude product, which
  7. customis then purified by column chromatography over silica gel (eluant: ethyl acetate/hexane=1:3)

출처 및 근거

ORD 기록
ord-dea33564835446dd8b51cdf17d8d936c
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06262058B1

반응 노트

불러오는 중…