Triethylamine → 3-(8-Azabicyclo[3.2.1]octan-8-yl)sulfonyl-1-dimethylcarbamoyl-1H-1,2,4-triazole

HRID 1293148

反応式

HRID 1293148 の反応式
Cl[S:2]([C:5]1[N:9]=[CH:8][N:7]([C:10](=[O:14])[N:11]([CH3:13])[CH3:12])[N:6]=1)(=[O:4])=[O:3].Cl.[CH:16]12[NH:23][CH:20]([CH2:21][CH2:22]1)[CH2:19][CH2:18][CH2:17]2.C(N(CC)CC)C>C(OCC)(=O)C>[CH:20]12[N:23]([S:2]([C:5]3[N:9]=[CH:8][N:7]([C:10](=[O:14])[N:11]([CH3:13])[CH3:12])[N:6]=3)(=[O:4])=[O:3])[CH:16]([CH2:22][CH2:21]1)[CH2:17][CH2:18][CH2:19]2

参加物

5

反応物 3

HCID 8471TriethylamineHCID 5222728-Azabicyclo[3.2.1]octane hydrochlorideHCID 178387483-chlorosulfonyl-1-dimethylcarbamoyl-1H-1,2,4-triazole

生成物 1

HCID 589054543-(8-Azabicyclo[3.2.1]octan-8-yl)sulfonyl-1-dimethylcarbamoyl-1H-1,2,4-triazole収率 24.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 3-chlorosulfonyl-1-dimethylcarbamoyl-1H-1,2,4-triazole (Example 54-a) (470 mg), 8-azabicyclo[3.2.1]octane hydrochloride (350 mg), triethylamine (0.7 ml), and ethyl acetate (10 ml) was stirred overnight at room temperature. The reaction solution was washed with water, followed by saturated aqueous sodium chloride solution, and concentrated. The residue was subjected to a silica-gel column chromatography with 50 to 100% ethyl acetate/hexane to yield the title compound (150 mg).

後処理

  1. washThe reaction solution was washed with water
  2. concentrationconcentrated

出典と根拠

ORDレコード
ord-808be267f9064c308abe3a533da335b4
出典データセット
uspto-grants-2007_07
特許番号
US07238720B2

関連ノート

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