تفاعل #42143

معادلة التفاعل

biphenyl-2-ylcarbamic acid 1-{2-[(4-hydroxymethyl-2-methoxybenzoyl)methylamino]ethyl}piperidin-4-yl ester

DMSO

DIPEA

→

Biphenyl-2-ylcarbamic acid 1-{2-[(4-formyl-2-methoxybenzoyl)methylamino]ethyl}piperidin-4-yl Ester

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONTo the solution was added sulfur trioxide-pyridine complex (240 mg, 15 mmol)
2. 2
   أخرىthe reaction mixture was quenched with water (˜3 mL)
3. 3
   أخرىTwo layers were separated
4. 4
   تجفيفthe organic layer was dried over MgSO4
5. 5
   ترشيحfiltered
6. 6
   أخرىthe title intermediate was used directly in the next reaction

الإجراء التجريبي

To a stirred solution of biphenyl-2-ylcarbamic acid 1-{2-[(4-hydroxymethyl-2-methoxybenzoyl)methylamino]ethyl}piperidin-4-yl ester (78 mg, 1.5 mmol; prepared as described in Preparation 20) in DCM (2.5 mL) at −15° C. was added DMSO (130 μL, 22.5 mmol), and DIPEA (130 μL, 7.5 mmol). To the solution was added sulfur trioxide-pyridine complex (240 mg, 15 mmol). After 30 minutes, the reaction mixture was quenched with water (˜3 mL). Two layers were separated, the organic layer was dried over MgSO4, filtered and the title intermediate was used directly in the next reaction.

المصدر