Dimethylformamide dimethyl acetal → 3,9-Dimethyl-beta-carboline
反応式
[CH3:1][C:2]1[N:3]=[CH:4][C:5]2[NH:6][C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3.[CH3:15]OC(OC)N(C)C.N1(C2CCCCCCC2)CCCCCCN1>CN(C)C=O>[CH3:1][C:2]1[N:3]=[CH:4][C:5]2[N:6]([CH3:15])[C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][CH:10]=[CH:9][CH:8]=3参加物
5
実験手順
0.182 g of 3-methyl-β-carboline (example 5), 0.5 ml of N,N-dimethylformamide-dimethylacetal (90%) and 0.02 g of diazabicyclooctane (Dabco) are stirred in 30 ml of absolute N,N-dimethylformamide for 15 hours at 110° C. The solvent is distilled off under vacuum and the residue is chromatographed on silica gel. (Methylene chloride/ethanol: 9+1). 0.095 g of 3,9-dimethyl-β-carboline with a 134° C. melting point (decomposition) is obtained.
後処理
- distillationThe solvent is distilled off under vacuum
- customthe residue is chromatographed on silica gel
- customwith a 134° C.
- customis obtained
出典と根拠
- ORDレコード
- ord-b8750ec4c71049779173d6fd74688f96
- 出典データセット
- uspto-grants-1988_03
- 特許番号
- US04731358
反応ノート
読み込み中…