Bromide ion → 2-Bromo-5,6,7,8-tetrahydro-4H-thiazolo[4,5-d]azepine
反応式
N(OC(C)(C)C)=O.[Br-:8].C(OC([N:16]1[CH2:22][CH2:21][C:20]2[S:23][C:24](N)=[N:25][C:19]=2[CH2:18][CH2:17]1)=O)(C)(C)C>C(#N)C>[Br:8][C:24]1[S:23][C:20]2[CH2:21][CH2:22][NH:16][CH2:17][CH2:18][C:19]=2[N:25]=1参加物
5
実験手順
238 μl tert.-butyl nitrite was added to 447 mg cupper (II) bromide in 50 mL acetonitrile. The reaction was stirred 10 min. at RT and then 270 mg 2-amino-4,5,7,8-tetrahydro-thiazolo[4,5-d]-azepine-6-carboxylic acid tert-butyl ester was added. The reaction was stirred 30 min. at 60° C. The reaction was purified by HPLC. The residue was dissolved in 10 mL dichlormethane and 10 mL trifluor acetic acid and stirred at RT for 1 h. The mixture was evaporated to give 112 mg of the desired product. Rt: 0.92 min (method I), (M+H)+: 233/235
後処理
- stirringThe reaction was stirred 30 min. at 60° C
- customThe reaction was purified by HPLC
- dissolutionThe residue was dissolved in 10 mL dichlormethane
- stirring10 mL trifluor acetic acid and stirred at RT for 1 h
- customThe mixture was evaporated
出典と根拠
- ORDレコード
- ord-1470513fd5de4268aafeba34a15090b7
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642774B2
反応ノート
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