Cyanogen Bromide → HCID 13392479、化合物
反応式
[Cl:1][C:2]1[C:12]2[CH2:11][CH2:10][N:9]([CH3:13])[CH2:8][CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[N:14]#CBr>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:12]2[CH2:11][CH2:10][N:9]([C:13]#[N:14])[CH2:8][CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
A stirred solution of 1.2 g. of 6-chloro-3-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine in 30 ml. of toluene was treated at 50° by dropwise addition with a solution of 0.7 g. cyanogen bromide in 25 ml. of toluene. Following the addition, the mixture was stirred and heated at 50° for one hour. A stream of nitrogen was passed over the surface of the solution during the reaction. The mixture was cooled, filtered and the filtrate concentrated in vacuo to yield 6-chloro-3-cyano-2,3,4,5-tetrahydro-1H-3-benzazepine melting at 81°-82° from hexane-ether solution.
後処理
- additionthe addition
- temperatureheated at 50° for one hour
- customA stream of nitrogen was passed over the surface of the solution during the reaction
- temperatureThe mixture was cooled
- filtrationfiltered
- concentrationthe filtrate concentrated in vacuo
出典と根拠
- ORDレコード
- ord-a4c454f5a33a4e32af9e5bf54f8064ad
- 出典データセット
- uspto-grants-1985_01
- 特許番号
- US04496558
反応ノート
読み込み中…