反応 #657299

反応方程式

3

1-[(3-Oxo-2-oxa-bicyclo[2.2.1]heptane-5-carbonyl)-amino]-2-vinyl-cyclopropane carboxylic acid ethyl ester

DIPEA

water

→

2-(1-Ethoxycarbonyl-2-vinylcyclopropylcarbamoyl)-4-hydroxy-cyclopentane carboxylic acid diisopropylethylamine salt

反応条件

後処理

1. 1
   その他The reaction vessel was sealed
2. 2
   workup.STIRRINGAfter 1 min of pre-stirring
3. 3
   その他the reaction was irradiated for 40 min to a set temperature of 100° C
4. 4
   濃縮the transparent solution was concentrated in vacuo
5. 5
   その他to remove any residual water

実験手順

To a solution of 3 (800 mg, 2.73 mmol) in water (15 mL) in a 20 mL microwave reaction vessel was added DIPEA (1.2 mL, 6.8 mmol) and a stir bar. The reaction vessel was sealed and the immiscible slurry was shaken vigorously before insertion in the microwave oven cavity. After 1 min of pre-stirring, the reaction was irradiated for 40 min to a set temperature of 100° C. After cooling to 40° C., the transparent solution was concentrated in vacuo, and the residual brown oil co-evaporated 3 times with MeCN to remove any residual water. The crude product 4, in the form of a DIPEA salt, was immediately taken forward to the next step. LC/MS (Method A): tR=1.29 min, >95%, m/z (ESI+)=312 (MH+).

出典