Carbon Tetrachloride → 7-Chloromethyl-4-(3-thienyl)coumarin
反応式
O[CH2:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([C:14]3[CH:18]=[CH:17][S:16][CH:15]=3)=[CH:8][C:9](=[O:13])[O:10]2)=[CH:5][CH:4]=1.CN(C)P(N(C)C)N(C)C.C(Cl)(Cl)(Cl)[Cl:30]>C1COCC1.CCOCC>[Cl:30][CH2:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([C:14]3[CH:18]=[CH:17][S:16][CH:15]=3)=[CH:8][C:9](=[O:13])[O:10]2)=[CH:5][CH:4]=1参加物
6
実験手順
To a solution of the alcohol from Step 1 (1.65 g) and hexamethylphosphorous triamide in 35 mL THF at 0° C. was added CCl4 (1.3 mL) and the mixture stirred for 30 min. The mixture was diluted with Et2O, filtered, concentrated and the residue chromatographed (30% EtOAc/hexane) to provide the title compound as a solid, m.p. 125°-127° C.
後処理
- filtrationfiltered
- concentrationconcentrated
- customthe residue chromatographed (30% EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-41bf4b14ae7e4194a8b652aa27b29dc4
- 出典データセット
- uspto-grants-1995_06
- 特許番号
- US05424320
反応ノート
読み込み中…