Acetic Acid → 4-Hydroxy-2,3,5-trimethylbenzaldehyde

温度

115 °C

A mixture of 2,3,6-trimethylphenol (5 g, 0.036 mol) and hexamethylenetetramine (2.06 g, 0.0147 mol) in acetic acid (20 ml) was stirred at 115° C. for 2 hrs. The solvent (10 ml) was distilled and 20% (v/v) H2SO4 (20 ml) was added, and then the mixture was stirred at 115° C. for 20 min. The mixture was then poured on ice cold water (50 ml) and the separated solid was filtered, washed well with cold water (25 ml) and suck-dried. The wet cake was dried at 90° C. for 2 hrs under vacuum to yield 2,3,5-trimethyl-4-hydroxy-benzaldehyde (4.5 g, 75%; Table 1, no. 12).

1. distillationThe solvent (10 ml) was distilled
2. addition20% (v/v) H2SO4 (20 ml) was added
3. stirringthe mixture was stirred at 115° C. for 20 min
4. additionThe mixture was then poured on ice cold water (50 ml)
5. filtrationthe separated solid was filtered
6. washwashed well with cold water (25 ml)
7. customsuck-dried
8. customThe wet cake was dried at 90° C. for 2 hrs under vacuum

ORDレコード

ord-77f67864220348a6bc9a24e5108e2344

出典データセット

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08846982B2