Diisopropylethylamine → HCID 86680329, 화합물

To a solution of 3.99 g of Boc-L-alanine in 50 ml of DMF were added 12.02 g of HATU, 4.3 ml of Hünig's base and 5.00 g (R)-2-(4-Methoxy-benzylamino)-butyric acid methyl ester. The reaction was stirred overnight, and 6.01 g of HATU and 2.1 ml of Hünig's base were added, and the reaction was stirred for 24 h at r.t. and then for 4 h at 50° C. The reaction was poured unto water, the layers were separated and the aqueous phase was extracted with EtOAc twice. The combined organic layers war washed with 10% aqueous citric acid twice, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by flash chromatography (silica, heptane/EtOAc) to obtain 7.60 g (88%) of the title compound.

1. stirringthe reaction was stirred for 24 h at r.t.
2. waitfor 4 h at 50° C
3. customthe layers were separated
4. extractionthe aqueous phase was extracted with EtOAc twice
5. washThe combined organic layers war washed with 10% aqueous citric acid twice
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue was purified by flash chromatography (silica, heptane/EtOAc)

ORD 기록

ord-98d900e33a76413f839c554af2849a07

출처 데이터셋

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08686150B2