反応 #96175

反応方程式

2-Acetylthio-3-chlorobenzoic acid

N-cyclopentylglycine t-butyl ester

→

oil

収率 100.0%

N-(2-Acetylthio-3-chlorobenzoyl)-N-cyclopentylglycine t-butyl ester

収率 100.0%

溶媒

methylene chloride

methylene chloride

反応条件

後処理

1. 1
   ろ過The DCC-urea was filtered
2. 2
   洗浄washed with CH2Cl2
3. 3
   洗浄The filtrate was then washed 2×125 ml 1N HCl, 2×125 ml saturated NaHCO3, 2×125 ml brine
4. 4
   乾燥dried (MgSO4)
5. 5
   ろ過filtered
6. 6
   濃縮concentrated

実験手順

2-Acetylthio-3-chlorobenzoic acid (11.5 g, 50 mmol) and N-cyclopentylglycine t-butyl ester (10.0 g, 50 mmol) in methylene chloride (350 ml) were cooled to 0°-5° C., and N,N1 -dicyclohexylcarbodiimide (10.3 g, 50 mmol) in methylene chloride (50 ml) was added. The mixture was stirred overnight. The DCC-urea was filtered and washed with CH2Cl2. The filtrate was then washed 2×125 ml 1N HCl, 2×125 ml saturated NaHCO3, 2×125 ml brine, dried (MgSO4), filtered and concentrated to give 20.6 g of an oil. The crude product was used without further purification in the next step.

出典