تفاعل #167280

معادلة التفاعل

Sodium methoxide

1-(2-chloro-pyridin-4-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one

1-(2-Chloro-pyridin-4-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one

MeOH

→

product

المردود 30.6%

1-(2-Methoxy-pyridin-4-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one

المردود 30.6%

المذيبات

1,4-dioxane

CHCl3

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةmaintained at the same temperature for 4 days
2. 2
   workup.DISTILLATIONThe solvent was distilled from the reaction mixture
3. 3
   أخرىthe concentrate was partitioned between water and ethylacetate
4. 4
   تجفيفThe organic layer was dried over Na2SO4
5. 5
   أخرىto afford the crude product
6. 6
   أخرىPurification by column preparative HPLC

الإجراء التجريبي

Sodium methoxide (225 mg, 4.165 mmol) was added dropwise to a stirred solution of 1-(2-chloro-pyridin-4-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one (58A: 100 mg, 0.374 mmol) in 1,4-dioxane (20 mL) over a period of 10 minutes. The resulting mixture was heated to 110° C. and maintained at the same temperature for 4 days. The reaction was monitored by TLC (10% MeOH in CHCl3). The solvent was distilled from the reaction mixture and the concentrate was partitioned between water and ethylacetate. The organic layer was dried over Na2SO4 to afford the crude product. Purification by column preparative HPLC afforded 30 mg of the product (30.61% yield).

المصدر