Diisopropylethylamine → HCID 86653641, Verbindung

TBTU (3.22 mmol, 1.05 eq) is added to a solution of 2-amino-5-(3-fluoro-phenyl)-thiazole-4-carboxylic acid (3.07 mmol, 1.0 eq), N-[(1S,3S,5S)-2-aza-bicyclo[3.1.0]hex-3-ylmethyl]-2,2,2-trifluoro-acetamide (3.07 mmol, 1.0 eq) and DIPEA (9.20 mmol, 3.0 eq) in DCM (15 mL) and DMF (3.0 mL). After 2 h the mixture is washed twice with water, once with sat. aqueous NaHCO3 solution, once with hydrochloric acid (0.2 M) and three times with water. The organic layer is dried over Na2SO4, the solvents are removed in vacuo and the residue is purified by preparative TLC (DCM/MeOH 9/1) to give the desired product as an orange foam. LC-MS (acidic): tR=0.87 min; [M+H]+=429.1.

1. washAfter 2 h the mixture is washed twice with water, once with sat. aqueous NaHCO3 solution, once with hydrochloric acid (0.2 M) and three times with water
2. dry with materialThe organic layer is dried over Na2SO4
3. customthe solvents are removed in vacuo
4. customthe residue is purified by preparative TLC (DCM/MeOH 9/1)

ORD-Eintrag

ord-da8c4d191279490da31973d694078a9b

Quelldatensatz

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08288435B2