HCID 13823510, compound → HCID 13823511, compound

The ester oil from Part (1) (1.82 g, 9.6 mmol) was treated with 2N NaOH (20 ml). The heterogeneous mixture was stirred vigorously at room temperature and became homogeneous in about 30 minutes. After stirring 4 hours, the reaction was washed with ether (2×30 ml) and the ether washes were reextracted with 2N NaOH solution (10 ml). The combined aqueous layers were acidified to pH 1 with concentrated HCl and the product was extracted into ether (2×30 ml). The combined ether extracts were washed with saturated NaCl solution (2×20 ml), dried (MgSO4) and freed of solvent in vacuo. The crude solid obtained (1.48 g) was recrystallized from benzene to give title acid (1.11 g, 6.3 mmol, 66%) as colorless crystals, m.p. 83°-84°.

1. stirringAfter stirring 4 hours
2. washthe reaction was washed with ether (2×30 ml)
3. extractionthe product was extracted into ether (2×30 ml)
4. washThe combined ether extracts were washed with saturated NaCl solution (2×20 ml)
5. dry with materialdried (MgSO4)
6. customThe crude solid obtained (1.48 g)
7. customwas recrystallized from benzene
8. customto give title acid (1.11 g, 6.3 mmol, 66%) as colorless crystals, m.p. 83°-84°

ORD record

ord-7725991059014a3b92110e7666d4c08b

Source dataset

uspto-grants-1988_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04735962