Water → HCID 20492177、化合物
反応式
P(Cl)(Cl)(Cl)=O.[O:6]1[CH:10]=[CH:9][CH:8]=[C:7]1[CH2:11][S:12][CH2:13][CH2:14][N:15]1[C:23](=[O:24])[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16]1=[O:25].O.[CH:27]([OH:30])(C)C>CN(C)C=O>[CH:27]([C:10]1[O:6][C:7]([CH2:11][S:12][CH2:13][CH2:14][N:15]2[C:23](=[O:24])[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16]2=[O:25])=[CH:8][CH:9]=1)=[O:30]参加物
6
実験手順
A solution of phosphoryl chloride (21.4 g) in dry dimethylformamide (40 ml), cooled in ice, was added portionwise to a solution of N-[2-[(2-furanylmethyl)thio]ethyl]-1H-isoindole-1,3(2H)-dione (21.4 g) in dry dimethylformamide (70 ml). After 5 hours at room temperature, the solution was poured into iced water (1.7 l). Isopropyl alcohol (150 ml) was added and after 18 hours the solid which separated was filtered and crystallised from ethyl acetate-ether to give the title compound (22.3 g) m.p. 76°-77°.
後処理
- customseparated
- filtrationwas filtered
- customcrystallised from ethyl acetate-ether
出典と根拠
- ORDレコード
- ord-1eacc8d32d3c4d44976bc24771abbedd
- 出典データセット
- uspto-grants-1983_08
- 特許番号
- US04399294
反応ノート
読み込み中…