تفاعل #2160382

معادلة التفاعل

2,2,2-trichloroethyl chloroformate

5-amino-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one

5-Amino-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one

Proton Sponge

→

desired product

[3-Oxo-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-5-yl)carbamic acid, 2,2,2-trichloroethyl ester

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThis mixture was heated
2. 2
   درجة الحرارةat reflux for 16 hours
3. 3
   أخرىThe reaction mixture was quenched
4. 4
   workup.ADDITIONby pouring it into 200 ml of water
5. 5
   أخرىthe precipitate formed
6. 6
   ترشيحwas collected by filtration

الإجراء التجريبي

A 500 mg amount of 5-amino-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one (prepared as described in Example 29) was suspended and stirred in 25.0 ml of dry tetrahydrofuran, then 320 mg of [1,8-bis(dimethylamino)naphthalene,N,N, N',N'-tetramethyl-1,8-naphthalenediamine] (Proton Sponge®) was added followed by 0.207 ml of 2,2,2-trichloroethyl chloroformate. This mixture was heated at reflux for 16 hours. The reaction mixture was quenched by pouring it into 200 ml of water and the precipitate formed was collected by filtration to give 419 mg of the desired product as a white solid, m.p. 225°-226° C.

المصدر