Phosphorus oxychloride → 4-chloro-N-(3-(dimethylamino)propyl)-5-methylthieno[2,3-d]pyrimidine-6-sulfonamide hydrochloride salt

HRID 450588ノート

反応式

HRID 450588 の反応式
[CH3:1][N:2]([CH3:21])[CH2:3][CH2:4][CH2:5][NH:6][S:7]([C:10]1[S:19][C:13]2[N:14]=[CH:15][NH:16][C:17](=O)[C:12]=2[C:11]=1[CH3:20])(=[O:9])=[O:8].P(Cl)(Cl)([Cl:24])=O>>[ClH:24].[Cl:24][C:17]1[C:12]2[C:11]([CH3:20])=[C:10]([S:7]([NH:6][CH2:5][CH2:4][CH2:3][N:2]([CH3:21])[CH3:1])(=[O:9])=[O:8])[S:19][C:13]=2[N:14]=[CH:15][N:16]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 69669093HCID 69669093、化合物

生成物 1

HCID 866656674-chloro-N-(3-(dimethylamino)propyl)-5-methylthieno[2,3-d]pyrimidine-6-sulfonamide hydrochloride salt

実験手順

To N-(3-(dimethylamino)propyl)-5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-sulfonamide (0.6 g, 1.8 mmol) was added phosphorus oxychloride (5.0 mL, 36 mmol) and the suspension heated at reflux for 1.5 hours. The reaction was cooled to ambient temperature and the excess phosphorus oxychloride removed under vacuum. The residue was co-evaporated several times with chloroform. Drying under vacuum gave a hydroscopic cream solid that was used without further purification (0.65 g, 92%).

後処理

  1. temperaturethe suspension heated
  2. temperatureat reflux for 1.5 hours
  3. customthe excess phosphorus oxychloride removed under vacuum
  4. customDrying under vacuum
  5. customgave a hydroscopic cream solid that
  6. customwas used without further purification (0.65 g, 92%)

出典と根拠

ORDレコード
ord-c2872b3eba1e4f8ea82a1490421cd450
出典データセット
uspto-grants-2013_07
特許番号
US08486953B2

反応ノート

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