تفاعل #556549

معادلة التفاعل

sodium hydride

7-methyl-1,3-dihydro-indol-2-one

DMF

iodomethane

→

1,3,3,7-tetramethyl-1,3-dihydro-indol-2-one

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture was stirred for 2 h at RT
2. 2
   استخلاصit was extracted with DCM and aqueous sodium hydrogen carbonate solution
3. 3
   أخرىThe organic phase was dried on sodium sulphate
4. 4
   ترشيحfiltered
5. 5
   أخرىevaporated down i
6. 6
   أخرىThe residue was purified by preparative HPLC-MS
7. 7
   workup.ADDITIONThe fractions containing the product
8. 8
   أخرىfreeze-dried

الإجراء التجريبي

2.00 g (50.0 mmol) sodium hydride (55%, suspension in mineral oil) were added at 0° C. to 2.34 g (3.58 mmol) 7-methyl-1,3-dihydro-indol-2-one in 20 mL DMF and the mixture was stirred for 30 min. Then 3.00 mL (48.2 mmol) iodomethane were added and the mixture was stirred for 2 h at RT. Ice water was added to the reaction mixture, then it was extracted with DCM and aqueous sodium hydrogen carbonate solution. The organic phase was dried on sodium sulphate, filtered and evaporated down i. vac. The residue was purified by preparative HPLC-MS. The fractions containing the product were combined and freeze-dried.

المصدر