反応 #47838

反応方程式

propionyl chloride

propionyl chloride

triethylamine

1-Amino-6-methoxy-3-phenyl-1H-indene-2-carboxylic acid ethyl ester

1-amino-6-methoxy-3-phenyl-1H-indene-2-carboxylic Acid Ethyl Ester

→

titled compound

収率 50.0%

6-methoxy-3-phenyl-1-propionylamino-1H-indene-2-carboxylic Acid Ethyl Ester

収率 50.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   その他at 0° C
2. 2
   workup.STIRRINGto be stirred for 15 hrs
3. 3
   洗浄The resulting mixture was washed with saturated saline
4. 4
   抽出extracted with dichloromethane
5. 5
   その他The organic layer was separated
6. 6
   乾燥dried over anhydrous MgSO4
7. 7
   濃縮concentrated under a reduced pressure
8. 8
   その他The resulting residue was purified by flash chromatography

実験手順

1-Amino-6-methoxy-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (50 mg, 0.16 mmol) prepared in Example 20 was dissolved in dichloromethane (10 mL), and propionyl chloride (150.38 mg, 0.14 mL, 1.62 mmol) and triethylamine (180.12 mg, 0.25 mL, 1.78 mmol) were added thereto in order at 0° C. The mixture was stirred for 24 hrs at RT, and an excess amount of propionyl chloride (2 mL) was further added thereto to be stirred for 15 hrs. The resulting mixture was washed with saturated saline and extracted with dichloromethane. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 29 mg of the titled compound (yield: 50%).

出典