Diethyl Ether → HCID 20536237, compound
Reaction equation
[C:1]([C:3]1[CH:4]=[CH:5][C:6]([OH:14])=[C:7]([C:9]([CH3:13])([CH3:12])[CH2:10][OH:11])[CH:8]=1)#[N:2].C(OCC)C.CO[C:22](OC)([CH3:24])[CH3:23]>S(=O)(=O)(O)O>[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[O:14][C:22]([CH3:24])([CH3:23])[O:11][CH2:10][C:9]([CH3:12])([CH3:13])[C:7]=2[CH:8]=1)#[N:2]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
A suspension of 2-(5-cyano-2-hydroxyphenyl)-2-methyl-1-propanol (5 g), prepared as in Example 26, in 2,2-dimethoxypropane was treated with 2 drops sulphuric acid at 10° C. After 1 hour at ambient temperature, diethyl ether was added, and the solution was washed with sodium hydroxide solution and water (twice). It was then dried over magnesium sulphate and run down, yielding 2.4 g of an oil which solidified on standing. The solid was dissolved in petroleum ether (bp 40°-60° C.) and the solution was cooled in an ice/salt bath. The resulting crystalline solid was separated off by filtration, yielding 1.9 g of product, mp 55°-56° C.
Workup
- washthe solution was washed with sodium hydroxide solution and water (twice)
- dry with materialIt was then dried over magnesium sulphate
Sources & evidence
- ORD record
- ord-b90d2269cf5a4f718646cb12cfee1a8f
- Source dataset
- uspto-grants-1981_04
- Patent number
- US04263037
Reaction notes
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