反応式
CO[C:3]1[C:12]2[C:7](=[C:8](C)[C:9]3[NH:15][C:14]4[CH:16]=[CH:17][N:18]=[CH:19][C:13]=4[C:10]=3[CH:11]=2)[CH:6]=[CH:5][N:4]=1.[I-].[Na+].C[Si](Cl)(C)C.C[Si](C)(C)N[Si](C)(C)C.C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:48]([N:50]([CH2:53][CH2:54][CH2:55][NH2:56])[CH2:51][CH3:52])[CH3:49]>C(#N)C>[CH2:48]([N:50]([CH2:51][CH3:52])[CH2:53][CH2:54][CH2:55][NH:56][C:3]1[C:12]2[C:7](=[CH:8][C:9]3[NH:15][C:14]4[CH:16]=[CH:17][N:18]=[CH:19][C:13]=4[C:10]=3[CH:11]=2)[CH:6]=[CH:5][N:4]=1)[CH3:49]参加物
8
反応物 6
生成物 1
試薬・触媒・溶媒 1
実験手順
0.87 g (0.0033 mole) of 10-methoxy 6-methyl 5H-pyrido[3',4':4,5]pyrrolo[2,3-g]isoquinoline and 0.495 g (0.003 mole) of sodium iodide are suspended in 25 ml of acetonitrile and 4.2 ml (0.33 mole) of trimethylsilylchloride, and then heated at 40° C. for 17 hours. 10.5 ml (0.050 mole) of hexamethyldisilazane, 0.113 g (6×10-4 mole) of anhydrous p-toluenesulfonic acid and 22.4 ml (0.14 mole) of diethylaminopropylamine are then added. After distillation of the acetonitrile, the mixture is heated at reflux for 20 hours. It is evaporated to dryness under a partial vacuum and the residue is stirred with 20 ml of water and 5 ml of diisopropyl ether for 1 hour. The precipitate obtained is filtered off and dried under vacuum at 50° C.
後処理
- distillationAfter distillation of the acetonitrile
- temperaturethe mixture is heated
- temperatureat reflux for 20 hours
- customIt is evaporated to dryness under a partial vacuum
- customThe precipitate obtained
- filtrationis filtered off
- customdried under vacuum at 50° C.
出典と根拠
- ORDレコード
- ord-e86c1c5b169b4ebeb61e406073a700ff
- 出典データセット
- uspto-grants-1992_01
- 特許番号
- US05079363
関連ノート
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