반응식
[N+:1]([O-:4])(O)=[O:2].FC(F)(F)S(O)(=O)=O.[C:13]1([C:19]2[N:20]=[N:21][C:22]3[C:29]4([CH3:32])[CH2:30][CH2:31][CH:26]([C:27]([CH3:34])([CH3:33])[O:28]4)[C:23]=3[N+:24]=2[O-:25])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[OH2:2].[N+:1]([C:15]1[CH:14]=[C:13]([C:19]2[N:20]=[N:21][C:22]3[C:29]4([CH3:32])[CH2:30][CH2:31][CH:26]([C:27]([CH3:34])([CH3:33])[O:28]4)[C:23]=3[N+:24]=2[O-:25])[CH:18]=[CH:17][CH:16]=1)([O-:4])=[O:2]참가 물질
반응물 4
생성물 1
시약·촉매·용매 1
실험 절차
To a mixture of 0.2 ml. (0.005 mole) fuming nitric acid and 1.5 g. (0.01 mole) trifluoromethanesulfonic acid in 15 ml. anhydrous methylene chloride maintained at a temperature of -30° C. there is added dropwise a solution of 0.60 g. (0.002 mole) 3-phenyl-5,8-dihydro-6,6,8-trimethyl-5,8-ethano-6H-pyrano[4,3-e]-as-triazine-4-oxide in 15 ml. methylene chloride, maintaining the temperature at -30° C. throughout the addition. The resulting mixture is allowed to stir at ambient temperature for 72 hours, then poured onto ice and neutralized with solid sodium bicarbonate. The organic layer is removed, washed with saturated brine solution, dried over magnesium sulfate and evaporated. Trituration of the resulting residue with ether gives 3-(m-nitrophenyl)-5,8-dihydro-6,6,8-trimethyl-5,8-ethano-6H-pyrano[4,3-e]-as-triazine-4-oxide-monohydrate; m.p. 150° (d).
후처리
- additionTo a mixture of 0.2 ml
- additionthere is added dropwise a solution of 0.60 g
- additionthroughout the addition
- customThe organic layer is removed
- washwashed with saturated brine solution
- dry with materialdried over magnesium sulfate
- customevaporated
출처 및 근거
- ORD 기록
- ord-72ec76eb786049f3849d53a26b817876
- 출처 데이터셋
- uspto-grants-1980_10
- 특허 번호
- US04228280
연결된 노트
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