Chloromethyl Methyl Ether → HCID 11565322、化合物

Ethyldiisopropylamine (3.01 ml, 17.1 mmol) and methoxymethylchloride (1.5 ml, 15.7 mmol) were added to a dichloromethane solution (30 ml) of 5-bromo-2-hydroxy-3-methoxybenzaldehyde (3.3 g, 14.3 mmol) under ice cooling, and the mixture was stirred at room temperature for 2 hours. The reaction solution was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1→11:9). The purified product was concentrated to dryness under reduced pressure to obtain 5-bromo-3-methoxy-2-methoxymethoxybenzaldehyde (4.2 g) as light yellow solid.

1. washThe reaction solution was washed with water
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1→11:9)
5. concentrationThe purified product was concentrated to dryness under reduced pressure

ORDレコード

ord-6cb00748a0a0469c8784194f0d1e935e

出典データセット

uspto-grants-2011_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08071600B2