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

HRID 450588노트

반응식

HRID 450588 반응식
[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

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 69669093HCID 69669093, 화합물

생성물 1

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

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-c2872b3eba1e4f8ea82a1490421cd450
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486953B2

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