Formaldehyde → HCID 22368323、化合物
反応式
[Br:1][C:2]1[CH:12]=[CH:11][C:5]2[CH2:6][CH2:7][NH:8][CH2:9][CH2:10][C:4]=2[CH:3]=1.[CH2:13]=O>C(O)=O>[Br:1][C:2]1[CH:12]=[CH:11][C:5]2[CH2:6][CH2:7][N:8]([CH3:13])[CH2:9][CH2:10][C:4]=2[CH:3]=1参加物
4
反応条件
- 温度
- 70 °C
実験手順
2.43 g 7-Bromo-2,3,4,5-tetrahydro-1H-benzo[d]azepine are dissolved in 4.055 g of formic acid and 3.2 mL of formaldehyde solution was added. The mixture was stirred at 70° C. for 3.5 h and continued overnight at 25° C. The mixture was concentrated, diluted with water and 10 N NaOH to adjust to a basic pH. The mixture was then extracted with tertbutylmethylether (3×) and the organic phase dried (Na2SO4), filtered and concentrated to yield 2.48 g 7-bromo-3-methyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine as oil.
後処理
- waitcontinued overnight at 25° C
- concentrationThe mixture was concentrated
- additiondiluted with water and 10 N NaOH
- extractionThe mixture was then extracted with tertbutylmethylether (3×)
- dry with materialthe organic phase dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-05ded584c76347ee96bad8a19e398ff7
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08912173B2
反応ノート
読み込み中…