تفاعل #92253

معادلة التفاعل

DIEA

(R)-5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-amine

CDI

azetidin-3-ol hydrochloride

→

final product

المردود 100.0%

(R)—N-(5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-yl)-3-hydroxyazetidine-1-carboxamide

المردود 100.0%

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGAfter stirring for 5 minutes
2. 2
   تركيزthe reaction was concentrated
3. 3
   أخرىdirectly purified by reverse-phase column chromatography
4. 4
   غسيلeluting with 5 to 48% acetonitrile/water

الإجراء التجريبي

To a DCM (1.0 mL) solution of (R)-5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-amine (Preparation B; 50 mg, 0.16 mmol), was added CDI (39 mg, 0.24 mmol) at ambient temperature in one portion. After stirring two hours, azetidin-3-ol hydrochloride (35 mg, 0.32 mmol) [purchased from Oakwood] was added in one portion, followed by addition of DIEA (0.083 mL, 0.48 mmol). After stirring for 5 minutes, the reaction was concentrated and directly purified by reverse-phase column chromatography, eluting with 5 to 48% acetonitrile/water to yield the final product as a yellowish foamy powder (66 mg, 100% yield). MS (apci) m/z=415.2 (M+H).

المصدر