Acrylonitrile → HCID 86748707、化合物
反応式
[F:1][C:2]1[C:3]([OH:12])=[C:4]([C:7]([O:10][CH3:11])=[CH:8][CH:9]=1)[CH:5]=O.[C:13](#[N:16])[CH:14]=[CH2:15]>>[C:13]([C:14]1[CH2:15][O:12][C:3]2[C:4]([CH:5]=1)=[C:7]([O:10][CH3:11])[CH:8]=[CH:9][C:2]=2[F:1])#[N:16]参加物
3
実験手順
Crude 3-fluoro-hydroxy-6-methoxybenzaldehyde (8.0 g) from above, acrylonitrile (13 mL; 193 mmol) and 1,4. diazadicyclo [2,2,2]octane (0.66 g; 5.9 mmol) were refluxed in a three-necked round-bottom flask (50 mL) under nitrogen for 4 h. Rotary-evaporation of the volatiles left a thick, red oil which was flash-chromatographed on a silica column eluted with methylene chloride/n-hexane (4:5). Concentration of relevant fractions gave an impure product (91% GC) which was crystallized form EtOAc to give 1.31 g of the title compound as colourless bars. Mp. 133°-135° C.
後処理
- customRotary-evaporation of the volatiles
- waitleft a thick, red oil which
- customwas flash-chromatographed on a silica column
- washeluted with methylene chloride/n-hexane (4:5)
- customConcentration of relevant fractions gave an impure product (91% GC) which
- customwas crystallized form EtOAc
出典と根拠
- ORDレコード
- ord-17d34e57a95f455680653a34b67191a5
- 出典データセット
- uspto-grants-1997_06
- 特許番号
- US05639772
反応ノート
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