Methanol → HCID 67276724, compound
Reaction equation
[CH2:1](N(C(C)C)C(C)C)C.[SH:10][C:11]1C=[CH:15][CH:14]=[C:13](OC)[C:12]=1[OH:19].[CH3:20][OH:21]>>[SH:10][C:11]1[C:20]([O:21][CH3:1])=[CH:15][CH:14]=[CH:13][C:12]=1[OH:19]Participants
4
Procedure
N-ethyldiisopropylamine (12.9 mL) and 2-mercapto-6-methoxyphenol (9.8 g) synthesized in Reference Example 8(4) were added in that order to a methanol (180 mL) solution of the compound obtained in the above (4), and stirred at room temperature for 14 hours. The reaction solvent was evaporated off under reduced pressure, the residue was dissolved in ethyl acetate, and extracted twice with distilled water. The organic layer was dried with magnesium sulfate, and the solvent was evaporated off under reduced pressure. The obtained residue was purified by NH silica gel column chromatography (chloroform 100%) to obtain the intended compound (28.7 g, 100%).
Sources & evidence
- ORD record
- ord-cd5ebdde862141a8b5f37157946380f6
- Source dataset
- uspto-grants-2012_04
- Patent number
- US08163770B2
Reaction notes
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