تفاعل #1449260

معادلة التفاعل

(E)-3-[4-(2-morpholin-4-yl-ethyl)-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl]acrylic acid tert-butyl ester

TFA

CH2Cl2

→

title compound

المردود 96.0%

(E)-3-[4-(2-Morpholin-4-yl-ethyl)-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl]acrylic acid hydrochloride

المردود 96.0%

ظروف التفاعل

المعالجة

1. 1
   تركيزthe clear tan solution was concentrated in vacuo
2. 2
   workup.ADDITIONThe resulting oil was treated with anhydrous HCl (4 mL of a 4.0 M solution in dioxane, 16 mmol) and
3. 3
   أخرىthen sonicated for 15 min
4. 4
   workup.ADDITIONThe mixture was diluted with Et2O
5. 5
   أخرىsonicated for 10 min
6. 6
   أخرىThe solid was isolated by filtration
7. 7
   غسيلwashed with Et2O
8. 8
   أخرىdried under vacuum at 50° C. for 4.5 hr

الإجراء التجريبي

A solution of (E)-3-[4-(2-morpholin-4-yl-ethyl)-2-oxo-2,3,4,5-tetrahydro-1H-pyrido[2,3-e][1,4]diazepin-7-yl]acrylic acid tert-butyl ester (92 mg, 0.23 mmol) in CH2Cl2 (2 mL) was treated with TFA (2 mL). After stirring at room temperature for 30 min, the clear tan solution was concentrated in vacuo. The resulting oil was treated with anhydrous HCl (4 mL of a 4.0 M solution in dioxane, 16 mmol) and then sonicated for 15 min. The mixture was diluted with Et2O and sonicated for 10 min. The solid was isolated by filtration, washed with Et2O and dried under vacuum at 50° C. for 4.5 hr to give the title compound (0.10 g, 96%) as an off-white solid: MS (ESI) m/e 347 (M+H)+.

المصدر