Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-Amino-4-chloro-6-methyl-10,10-dioxo-10,11-dihydro-5-oxa-10lambda *6*-thia-dibenzo[a,d]cycloheptene-8-carboxylic acid | HCID 11631717 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 23673467 | HCID 23673467 | — |
Reaction Steps
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%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07964631B2 |
|---|
| Source dataset | uspto-grants-2011_06 |
|---|
| ORD ID | ord-9672674ae37c4f3eb85a40e88d22fda8 |
|---|
| Source note | uspto-grants-2011_06 |
|---|
