Sodium Hydroxide → HCID 12561502, compound
Reaction equation
C[O:2][C:3]([C:5]1[O:10][C:9]2[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[S:13][CH2:14][C:8]=2[C:7](=[O:19])[C:6]=1[CH3:20])=[O:4].[OH-].[Na+]>CO>[CH3:20][C:6]1[C:7](=[O:19])[C:8]2[CH2:14][S:13][C:12]3[CH:15]=[CH:16][CH:17]=[CH:18][C:11]=3[C:9]=2[O:10][C:5]=1[C:3]([OH:4])=[O:2]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 3-methyl-4-oxo-4H,5H-[1]benzothiopyrano[4,3-b]pyran-2-carboxylic acid methyl ester (1.60 g, 5.56 mmoles, described in Example 7) in a solution of sodium hydroxide (0.5 g) in methanol (50 ml is refluxed for 2 hr and evaporated. The residue is dissolved in water, and the solution is washed with diethyl ether and added with stirring to 3 N hydrochloric acid (25 ml). The fine precipitate is collected, washed with very dilute hydrochloric acid, small amount of water and then dried (1.506 g), mp 299°-301° C. The precipitate is crystallized from dimethyl sulfoxide-water to obtain crystals of the title compound, mp 302°-303° C.
Workup
- temperatureis refluxed for 2 hr
- customevaporated
- dissolutionThe residue is dissolved in water
- washthe solution is washed with diethyl ether
- additionadded
- customThe fine precipitate is collected
- washwashed with very dilute hydrochloric acid, small amount of water
- customdried (1.506 g), mp 299°-301° C
- customThe precipitate is crystallized from dimethyl sulfoxide-water
Sources & evidence
- ORD record
- ord-d7195fb22d7349ef85e954f16194be85
- Source dataset
- uspto-grants-1980_04
- Patent number
- US04198426
Reaction notes
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