Triethylamine → HCID 11848815, 화합물

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 기록

ord-b62ed1aa3362450ca5e8c03a72c217f2

출처 데이터셋

uspto-grants-2009_01

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07479488B2