1-Hydroxybenzotriazole → 4-(2-Oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylic acid-[1-(3,4-diethyl-benzyl)-2-(1'-methyl-4,4'-bipiperidinyl-1-yl)-2-oxo-ethyl]-amide

温度

40 °C

0.3 mL of triethylamine, 323 mg (1.01 mmol) of TBTU, 155 mg (1.01 mmol) of HOBt and 184 mg (1.01 mmol) of methyl-[4,4′]bipiperidinyl were added to a solution of 500 mg (1.02 mmol) of 3-(3,4-diethyl-phenyl)-2-{[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carbonyl]-amino}-propionic acid in 50 mL of THF and stirred for 4 h at RT and 2 h at 40° C. The reaction mixture was evaporated down, the residue was stirred with 40 mL of saturated NaHCO3 solution, the precipitated product was suction filtered, washed twice with water and triturated with EtOH. The white substance precipitated was suction filtered and washed twice with diethyl ether.

1. customThe reaction mixture was evaporated down
2. stirringthe residue was stirred with 40 mL of saturated NaHCO3 solution
3. filtrationfiltered
4. washwashed twice with water
5. customtriturated with EtOH
6. customThe white substance precipitated
7. filtrationfiltered
8. washwashed twice with diethyl ether

ORDレコード

ord-4ba66bfae60f48fd8cbe0ddd142c6f43

出典データセット

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07700589B2