Triethylamine → HCID 11848815、化合物

208 mg (0.82 mmol) ethyl [4,4′]bipiperidinyl-1-yl-acetate were added to a solution of 500 mg (0.82 mmol) of (R)-1-carboxy-2-(3,5-dibromo-4-hydroxy-phenyl)-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate, 315 mg (0.98 mmol) TBTU and 150 μL (1.06 mmol) triethylamine in 5 mL DMF and the reaction mixture was stirred overnight at RT. To complete the reaction a further 315 mg (0.98 mmol) TBTU, 150 μL (1.06 mmol) triethylamine and 208 mg (0.82 mmol) ethyl [4,4′]bipiperidinyl-1-yl-acetate were added and the mixture was again stirred overnight at RT. The reaction mixture was purified directly by HPLC without any further working up. The fractions containing the product were combined, evaporated down i.vac., neutralised with saturated NaHCO3 solution, the aqueous phase was extracted twice with 100 mL DCM and the combined organic phases were dried over Na2SO4. After the desiccant and solvent had been eliminated the residue was triturated with DIPE, suction filtered and dried in the air.

1. additionwere added
2. waitthe mixture was again stirred overnight at RT
3. customThe reaction mixture was purified directly by HPLC without
4. additionThe fractions containing the product
5. customevaporated down i.vac
6. extractionthe aqueous phase was extracted twice with 100 mL DCM
7. dry with materialthe combined organic phases were dried over Na2SO4
8. customwas triturated with DIPE, suction
9. filtrationfiltered
10. customdried in the air

ORDレコード

ord-2723aa2412204f4890a1e437442fa87e

出典データセット

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07700598B2