2-nitromethylenetetrahydro-2H-1,3-thiazine → 2-(5,6-Dihydro-4H-1,3-thiazin-2-yl)-N,N-dimethyl-2-nitroethen-1-amine
反応式
[N+:1]([CH:4]=[C:5]1[NH:10][CH2:9][CH2:8][CH2:7][S:6]1)([O-:3])=[O:2].CO[CH:13](OC)[N:14]([CH3:16])[CH3:15]>C(Cl)(Cl)Cl>[S:6]1[CH2:7][CH2:8][CH2:9][N:10]=[C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:13][N:14]([CH3:16])[CH3:15]参加物
4
実験手順
8.0 G OF TETRAHYDRO-2-(NITROMETHYLENE)-2H-1,3-thiazine, prepared as described in Example 2 of Ser. No. 554,361, 5.95 g of N,N-dimethylformamide dimethyl acetal and 25 ml of chloroform were mixed and the mixture was refluxed for about 16 hours. The solvent then was evaporated under reduced pressure to leave a dark orange solid. Recrystallization from ethyl acetate and methanol gave (1), as a light orange solid, m.p.: 168.5°-170°.
後処理
- temperaturethe mixture was refluxed for about 16 hours
- customThe solvent then was evaporated under reduced pressure
- customto leave a dark orange solid
- customRecrystallization from ethyl acetate and methanol
出典と根拠
- ORDレコード
- ord-8bb9d52282b845a8a9bd24360ae11130
- 出典データセット
- uspto-grants-1976_09
- 特許番号
- US03981871
反応ノート
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