Triethylamine → HCID 24860699, Verbindung

To a solution of 1-(2-methoxyethyl)-2-methyl-8-phenyl-1,6,7,8-tetrahydrochromeno[7,8-d]imidazole-5-carboxylic acid (200 mg, 0.55 mmol, Step 12), triethylamine (0.30 mL, 2.18 mmol), and O-benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium hexafluorophosphate (228 mg, 0.60 mmol) in N,N-dimethylformamide (5 mL) was added dimethylamine hydrochloride (49 mg, 0.60 mmol) at 0° C. After stirring at room temperature for 12 h, the mixture was poured onto water, and the aqueous layer was extracted with dichloromethane. The combined organic layer was dried over magnesium sulfate and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with dichloromethane/methanol (20:1) to afford the title compound as a white amorphous (215 mg, quant.).

1. additionthe mixture was poured onto water
2. extractionthe aqueous layer was extracted with dichloromethane
3. dry with materialThe combined organic layer was dried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane/methanol (20:1)

ORD-Eintrag

ord-95867aac19084ab5945ca30112d5a53f

Quelldatensatz

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08466166B2