3-(2-Nitroethenyl)thiophene → HCID 53948007、化合物
反応式
[N+:1]([CH:4]=[CH:5][C:6]1[CH:10]=[CH:9][S:8][CH:7]=1)([O-:3])=[O:2].[CH3:11][Al](C)C>CCCCCC>[N+:1]([CH2:4][CH:5]([C:6]1[CH:10]=[CH:9][S:8][CH:7]=1)[CH3:11])([O-:3])=[O:2]参加物
4
反応条件
- 温度
- 5 °C
実験手順
When R2 was H, the 3-(2-nitroethenyl)thiophene (1 eq) was suspended in hexane, cooled to 5° C. in an ice bath under nitrogen and slowly treated with 2N trimethylaluminum in hexane (2.6 eq). After 30 min, the solution was quenched with 3N HCl, diluted with ether and filtered. The organic layer was dried (Na2SO4) and condensed under reduced pressure to afford the crude product. This material was purified by flash silica gel column chromatography using 70% hexane in CH2Cl2. The product was obtained as a colorless oil (80%); MH+ at m/z 172.
後処理
- customthe solution was quenched with 3N HCl
- additiondiluted with ether
- filtrationfiltered
- customThe organic layer was dried
- custom(Na2SO4) and condensed under reduced pressure
- customto afford the crude product
- customThis material was purified by flash silica gel column chromatography
出典と根拠
- ORDレコード
- ord-378bf1916669437f84ca5c4c053f01c7
- 出典データセット
- uspto-grants-1994_03
- 特許番号
- US05294621
反応ノート
読み込み中…