Hydrogen Sulfide → HCID 88428340, compound

The crude material of (2S,3S)-dimethyl-3-ethylaspartate hydrobromide (27.2 g) of Example 6 was suspended in water (200.0 mL) and filtered. The filter cake was washed with water (300.0 mL) 2nd the combined aqueous solution were diluted with methanol (500.0 mL). To this solution was added copper(II) carbonate copper(II) hydroxide (76.4 g, 345.5 mmol) and the resulting green suspension was mechanically stirred in a Morton flask (2.0 L) for 119 h. The suspension was saturated with hydrogen sulfide for 1 h, then the resulting black suspension was filtered through celite. The filter cake was washed with an aqueous solution of methanol (70%, 1800.0 mL). The combined filtrate and washings were concentrated in vacuo to give the amino acid salt (19.6 g) which was used for further reaction without purification.

1. filtrationfiltered
2. washThe filter cake was washed with water (300.0 mL) 2nd the combined aqueous solution
3. additionwere diluted with methanol (500.0 mL)
4. filtrationthe resulting black suspension was filtered through celite
5. washThe filter cake was washed with an aqueous solution of methanol (70%, 1800.0 mL)
6. concentrationThe combined filtrate and washings were concentrated in vacuo

ORD record

ord-b6378de493184479809213b7a4612b7e

Source dataset

uspto-grants-1994_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05322942