Dichloromethane → 3,5-Dibromo-2-chloropyrazine
反応式
[Br:1][C:2]1[C:3](N)=[N:4][CH:5]=[C:6]([Br:8])[N:7]=1.N(OC(C)(C)C)=O.[Cl:17]CCl>[Ti](Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[C:3]([Cl:17])=[N:4][CH:5]=[C:6]([Br:8])[N:7]=1参加物
5
実験手順
To a solution of 3,5-dibromopyrazin-2-amine (1.00 g, 3.95 mmol) in dichloromethane 6.0 ml at 0° C. was added titanium tetrachloride (1 mol/l) in dichloromethane (3.95 mL, 3.95 mmol) then tert-butyl nitrite (1.05 mL, 7.91 mmol) was added dropwise. The reaction was warmed to RT then 1 more equivalent of TiCL4 was added and stirred for 1 h. The reaction was quenched with water and extracted with DCM. The organic layers was dried with sodium sulfate, filtered, and concentrated in vacuum. The crude product was carried to next step. MS (ESI) m/z: 272.2.
後処理
- addition1 more equivalent of TiCL4 was added
- customThe reaction was quenched with water
- extractionextracted with DCM
- dry with materialThe organic layers was dried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuum
出典と根拠
- ORDレコード
- ord-7aed7c16ee7542eb8f1c3f5607bec920
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434725B2
反応ノート
読み込み中…