反応式
O[CH2:2][C:3]1[O:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)=[CH:6][CH:7]=1.S(Br)([Br:20])=O>CN(C)C=O>[Br:20][CH2:2][C:3]1[O:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)=[CH:6][CH:7]=1参加物
4
実験手順
The hydroxymethyl compound (4.84 g; 0.02 mole) prepared in (a) above, was dissolved in dimethylformamide (30 ml) cooled to 0°-5° C. and thionyl bromide (1.7 ml; 0.02 mole) was added dropwise with stirring. After 2 hours the greenish-yellow solution was poured onto ice/water and extracted via diethyl ether. The ether extract was washed with NaCl (saturated solution) dried over molecular sieve 3A and evaporated to give a light brown oil which slowly crystallised (4.6 g).
後処理
- temperaturecooled to 0°-5° C.
- additionAfter 2 hours the greenish-yellow solution was poured onto ice/water
- extractionextracted via diethyl ether
- extractionThe ether extract
- washwas washed with NaCl (saturated solution)
- dry with materialdried over molecular sieve 3A
- customevaporated
- customto give a light brown oil which
- customslowly crystallised (4.6 g)
出典と根拠
- ORDレコード
- ord-33ac89cf71744453914d7bc31feff290
- 出典データセット
- uspto-grants-1978_10
- 特許番号
- US04123529
関連ノート
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