تفاعل #8225

معادلة التفاعل

7-nitrogramine

Dimethylsulfate

Sodium methoxide

→

3-(2-nitro-2-methylpropyl)-7-nitroindole

المردود 131.0%

المذيبات

2-nitropropane

methanol

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture is stirred overnight at room temperature
2. 2
   أخرىThe reaction is quenched by addition of saturated NH4Cl solution and ethyl acetate
3. 3
   استخلاصThe aqueous layer is extracted with ethyl acetate
4. 4
   غسيلthe combined organic layers are washed with brine
5. 5
   تجفيفdried over Na2SO4

الإجراء التجريبي

The 7-nitrogramine salt (2.0 g, 5.8 mmol) is suspended in a mixture of 2-nitropropane (9.5 mL) and methanol (9.5 mL). Dimethylsulfate (1.09 mL, 11.5 mmol) is added dropwise via syringe, and the resulting yellow solution is stirred at room temperature for 5 minutes. Sodium methoxide (0.62 g, 11.5 mmol) is then added in one portion, and the mixture is stirred overnight at room temperature. The reaction is quenched by addition of saturated NH4Cl solution and ethyl acetate. The aqueous layer is extracted with ethyl acetate, and the combined organic layers are washed with brine, and dried over Na2SO4 to give 1.0 g of 3-(2-nitro-2-methylpropyl)-7-nitroindole (69%).

المصدر