Imidazole → HCID 433777、化合物

To a solution of imidazole (1.23 g) and 1,1-bis(4-trifluoromethoxyphenyl)-1-hydroxy-2-(2H-tetrazol-2-yl)propane prepared as described in Example b 3 (1.34 g) in dry acetonitrile (50 ml) under an atmosphere of nitrogen, was added thionylchloride (1.07 g). A precipitate appeared and the reaction was stirred at room temperature for 5 hours. The mixture was then poured into water (100 ml) and extracted with ether (2×70 ml). The organic extracts were combined and washed well with saturated aqueous sodium bicarbonate solution (50 ml) then with water (50 ml). The organic layer was dried over anhydrous magnesium sulphate, and evaporated to give a yellow oil which was purified by h.p.l.c. on a silica gel column eluted with n-hexane/ethyl acetate (5:1) to give a colourless oil (900 mg).

1. extractionextracted with ether (2×70 ml)
2. washwashed well with saturated aqueous sodium bicarbonate solution (50 ml)
3. dry with materialThe organic layer was dried over anhydrous magnesium sulphate
4. customevaporated
5. customto give a yellow oil which
6. customwas purified by h.p.l.c
7. washon a silica gel column eluted with n-hexane/ethyl acetate (5:1)

ORDレコード

ord-80ed38b108544eaaba6ea72d56db83f8

出典データセット

uspto-grants-1989_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04829074