Sodium Hydroxide → HCID 23673467, compound
Reaction equation
[OH-].[Na+:2].[NH2:3][C:4]1[CH:24]=[C:23]([Cl:25])[C:7]2[O:8][C:9]3[C:18]([CH3:19])=[CH:17][C:16]([C:20]([OH:22])=[O:21])=[CH:15][C:10]=3[S:11](=[O:14])(=[O:13])[CH2:12][C:6]=2[CH:5]=1>O.CO>[Na+:2].[NH2:3][C:4]1[CH:24]=[C:23]([Cl:25])[C:7]2[O:8][C:9]3[C:18]([CH3:19])=[CH:17][C:16]([C:20]([O-:22])=[O:21])=[CH:15][C:10]=3[S:11](=[O:13])(=[O:14])[CH2:12][C:6]=2[CH:5]=1Participants
5
Conditions
- Temperature
- 25 °C
Procedure
A solution of sodium hydroxide (0.018 g, 0.47 mmol) in water (0.2 mL) was added to a solution of Example 2 (0.167 g, 0.47 mmol) in methanol (5 mL) and stirred at 25° C. for 15 min. The solvent was removed under vacuum, and dried to obtain the title compound. Yield: 0.16 g, (91%); 1H NMR (DMSO-d6, 300 MHz): δ 2.55 (s, 3H, CH3), 4.92 (s, 2H, CH2), 5.57 (s, 2H, NH2), 6.60 (m, 2H, Ar), 7.90 (s, 1H, Ar), 8.10 (s, 1H, Ar); MS: m/e (ES−) 352 (M−Na); analysis: C15H11ClNNaO5S.2H2O requires C, 43.75; H, 3.67; N, 3.40; Cl, 8.61; S, 7.79. found: C, 44.20; H, 3.34; N, 3.49; Cl, 9.25; S, 8.36%.
Workup
- customThe solvent was removed under vacuum
- customdried
Sources & evidence
- ORD record
- ord-9672674ae37c4f3eb85a40e88d22fda8
- Source dataset
- uspto-grants-2011_06
- Patent number
- US07964631B2
Reaction notes
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