Sodium → HCID 11357207、化合物

HRID 1384858ノート

反応式

HRID 1384858 の反応式
[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]

参加物

4

反応物 2

HCID 5360545SodiumHCID 18434022HCID 18434022、化合物

生成物 1

HCID 11357207HCID 11357207、化合物収率 106.2%

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-dea33564835446dd8b51cdf17d8d936c
出典データセット
uspto-grants-2001_07
特許番号
US06262058B1

反応ノート

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