1,1-Dimethylhydrazine → HCID 54468337、化合物
反応式
[CH3:1][O:2][C:3](=[CH2:6])[CH:4]=O.[CH3:7][N:8]([CH3:10])[NH2:9]>CCOCC>[CH3:1][O:2][C:3]([CH:4]=[N:9][N:8]([CH3:10])[CH3:7])=[CH2:6]参加物
4
実験手順
6.4 g of 2-methoxyacrolein are stirred for 1 hour at 30°-35° C. with 4.4 g of N,N-dimethylhydrazine in 50 ml of ether, dried at 20° C. with Na2SO4 and then the solvent is removed. Distillation at 74°-76° C./13 mbar gives 6.2 g of pure 2-methoxy-4-dimethylamino-4-azabutadiene. (b) 10.8 g of 2-methoxy-4-dimethylamino-4-azabutadiene and 15 g of 2-tert.-butylisothiazolin-3-one-1,1-dioxide are stirred for 11/2 h at 80°-85° C. in 250 ml of toluene. The crude bicyclic compound of formula IVb is further processed in the crude state as described in Example 4. ##STR16## The compounds listed in Table 1 are obtained in an analogous manner.
後処理
- dry with materialdried at 20° C. with Na2SO4
- customthe solvent is removed
- distillationDistillation at 74°-76° C./13 mbar
出典と根拠
- ORDレコード
- ord-e749b4b34a7b450e86acbdbeed1004cb
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04889933
反応ノート
読み込み中…