Preparation of moss acid_Kain Industrial Additive

Background and overview^[1]

Cosmic acid (2,4-dihydroxy-6-methylbenzoic acid) is a dihydroxybenzoic acid derivative with one more methyl group in its structure. It can be used as a pharmaceutical synthesis intermediate.

Preparation^[1]

The steps of the preparation method of Agophylla spp.

1) Add 60 to 98% industrial ethanol or methanol to the crushed Herbaceae (passed through a 20-80 mesh sieve), and perform cold soaking, ultrasonic or microwave extraction. The extraction time is 30 minutes to 7 days. The material-to-liquid ratio is 1:1~1:10;

2) Filter and recover the extract of Herbaceae under reduced pressure to obtain the total extract, add water to suspend, extract with petroleum ether, ethyl acetate and n-butanol in sequence, recover under reduced pressure to obtain the petroleum ether part and ethyl acetate respectively. Ester part and n-butanol part;

3) Repeat silica gel column chromatography on the determined active site, that is, the ethyl acetate part; petroleum ether: acetone (30:1) to obtain compound (1), chloroform: acetone (20:1) to obtain compound (2) ), compound (3) and compound (4) were obtained by thin layer preparation of chloroform: methanol (6:1), compound (5) was obtained by petroleum ether: acetone (15:1), compound (5) was obtained by chloroform: acetone (30:1) (6), chloroform: acetone (10:1) gives compound (7), chloroform: acetone (30:1) gives compound (8), chloroform: acetone (10:1) gives compound (9), chloroform: acetone ( 10:1) to obtain compound (10).

4) A variety of spectral and spectroscopic techniques (IR, UV, HR-ESIMS, EI-MS, 1D/2DNMR) were comprehensively used to identify the structures of the purified compounds, which were 8 phenolic acid compounds and 2 steroidal compounds, namely 4-methyl-2,6-dihydroxybenzaldehyde (1), β-orcinolate methyl ester (2), (+)-usnic acid (3) and (- )-Usnic acid (4), 5α, 8α-peroxyergodoster-6, 22E-diene-3βol (5), 5α, 8α-peroxyergodoster-6, 9 (11), 22E -Triene-3β-ol (6), leucoacetic acid (7), leucosaccharic acid methyl ester (8), citrienzoic acid ethyl ester (9), tea pickling acid (10), the measurement results are reliable.

Main reference materials

[1] CN200710307291.9 Preparation method of Alpinia alba extract