Hydrochloric Acid → 4-nitrosomorpholine-3-carboxylic Acid

Temperatur

0 °C

To a solution of morpholine-3-carboxylic acid (6.96 g, 52 mmol) in water (20 ml), at 0° C. under nitrogen, was added concentrated hydrochloric acid (4 ml), followed by sodium nitrite (5.0 g, 72 mmol) in small portions. The mixture was stirred at 0° C. for 1 hr, and then concentrated under vacuum at 30 to 35° C. The residue was stirred with 200 ml of acetone and filtered. The filtrate was evaporated and the residue treated with 50 ml of THF and concentrated. The process was repeated with 2×50 ml of THF to give 11.87 g of light yellow foam; MS (ESI) m/z 159.2 (M−H).

1. concentrationconcentrated under vacuum at 30 to 35° C
2. stirringThe residue was stirred with 200 ml of acetone
3. filtrationfiltered
4. customThe filtrate was evaporated
5. additionthe residue treated with 50 ml of THF
6. concentrationconcentrated

ORD-Eintrag

ord-6f440ab73b0d415aa706bec5f2368507

Quelldatensatz

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07812014B2