反応 #61716

反応方程式

(3S)-3-amino-1-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethyl]pyrrolidin-2-one

Intermediate 40

(3S)-3-amino-1-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethyl]pyrrolidin-2-one

5-chloro-1-benzofuran-2-sulfonyl chloride

Intermediate 51

5-chloro-1-benzofuran-2-sulfonyl chloride

ammonium chloride

→

title compound

収率 55.1%

5-Chloro-N-{(3S)-1-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethyl]-2-oxopyrrolidin-3-yl}-1-benzofuran-2-sulfonamide

収率 55.1%

溶媒

acetonitrile

acetonitrile

pyridine

反応条件

後処理

1. 1
   濃縮The mixture was concentrated under reduced pressure
2. 2
   その他the residue partitioned between chloroform and hydrochloric acid (2M)
3. 3
   洗浄The organic layer was washed with saturated sodium bicarbonate and brine
4. 4
   その他The organic layer was isolated
5. 5
   乾燥dried (over magnesium sulphate)
6. 6
   濃縮concentrated under reduced pressure

実験手順

To a solution of (3S)-3-amino-1-[(1S)-1-methyl-2-morpholin-4-yl-2-oxoethyl]pyrrolidin-2-one [Intermediate 40] (0.077 g) in anhydrous acetonitrile (2 ml) were added 5-chloro-1-benzofuran-2-sulfonyl chloride [Intermediate 51] (0.043 g) in acetonitrile (2 ml) and pyridine (0.057 ml), and the mixture was stirred at room temperature for 72 h. Saturated ammonium chloride solution (2 ml) was added and the resultant mixture stirred at room temperature for 20 min. The mixture was concentrated under reduced pressure and the residue partitioned between chloroform and hydrochloric acid (2M). The organic layer was washed with saturated sodium bicarbonate and brine. The organic layer was isolated, dried (over magnesium sulphate) and concentrated under reduced pressure to give the title compound (0.043 g) as a white solid.

出典