反応 #169670

ord-3733038fe77a4ef3b693f11951fb0d39

反応方程式

O=C(O)c1cccnc1
niacin
COC(=O)[C@@H]1CCCN1
L-proline methyl ester
CN1CCOCC1
N-methyl morpholine
CCN=C=NCCCN(C)C.Cl
EDC.HCl
COC(=O)C1CCCN1C(=O)c1cccnc1
product
収率 172.9%
COC(=O)C1CCCN1C(=O)c1cccnc1
1-(pyridine-3-carbonyl)-pyrrolidine-2-carboxylic acid methyl ester
収率 172.9%

溶媒

反応条件

温度
25°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with water (2×100 mL)
  2. 2
    乾燥dried over sodium sulphate
  3. 3
    その他Solvent was evaporated under reduced pressure

実験手順

To a solution of niacin (0.4 g 3.50 mmol) in DCM (10 mL) were added L-proline methyl ester (0.5 g, 3.21 mmol), N-methyl morpholine (1.1 mL, 0.10.5 mmol), EDC.HCl (1.2 g, 6.4 mmol) and catalytic amount of DMAP at ice temperature (0° C.). The mixture was allowed to stir at room temperature (25° C.) over a period of 2 h. The resulting mixture diluted with DCM (100 mL) washed with water (2×100 mL) and dried over sodium sulphate. Solvent was evaporated under reduced pressure to obtain product as yellow gummy oil (1.3 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08846721B2uspto-grants-2014_09