p-Methoxyphenylthionophosphine sulfide → Benzo-1,2,3-thiadiazole-7-thiocarboxamide
反応式
COC1C=CC(P(=S)=[S:10])=CC=1.[S:12]1[C:16]2[C:17]([C:21]([NH2:23])=O)=[CH:18][CH:19]=[CH:20][C:15]=2[N:14]=[N:13]1>C1(C)C=CC=CC=1>[S:12]1[C:16]2[C:17]([C:21](=[S:10])[NH2:23])=[CH:18][CH:19]=[CH:20][C:15]=2[N:14]=[N:13]1参加物
4
実験手順
A suspension of 2.42 g of p-methoxyphenylthiono-phosphine sulfide and 1.79 g of benzo-1,2,3-thiadiazole-7-carboxamide in 95 ml of toluene is refluxed under a nitrogen atmosphere for 6 hours. The mixture is then evaporated in vacuon and the residue is suspended in ethyl acetate and filtered off. The filtrate is recrystallized from ethyl acetate/tetrahydrofuran with added active charcoal. 1.1 g of yellow crystals of melting point 129°-131° C. result.
後処理
- temperatureis refluxed under a nitrogen atmosphere for 6 hours
- customThe mixture is then evaporated in vacuon
- filtrationfiltered off
- customThe filtrate is recrystallized from ethyl acetate/tetrahydrofuran
- additionwith added active charcoal
出典と根拠
- ORDレコード
- ord-ed276ae7cf7e46749d6f50b6ed188934
- 出典データセット
- uspto-grants-1993_07
- 特許番号
- US05229384
反応ノート
読み込み中…