تفاعل #51413

معادلة التفاعل

CH2Cl2

bromomethyl acetate

5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one

Cs2CO3

→

5-amino-7-(methoxyacetyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one Hydrochloride

المذيبات

DMF

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling to 23° C. the mixture
2. 2
   غسيلwashed with several portions of brine
3. 3
   تجفيفdried over Na2SO4
4. 4
   أخرىThe title compound was purified by chromatography (SiO2, CHCl3)

الإجراء التجريبي

A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (1.03, 3.08 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (1.10 g, 3.39 mmol) and warmed to 60° C. To the reaction mixture was added bromomethyl acetate (0.321 ml, 3.39 mmol) (Aldrich) and stirring continued for 17 h. After cooling to 23° C. the mixture was diluted with CH2Cl2, washed with several portions of brine and dried over Na2SO4. The title compound was purified by chromatography (SiO2, CHCl3).

المصدر