HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → HCID 178483720, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59144118 | HCID 59144118 | — |
| Reactant | Methyl thiophene-2-carbimidothioate hydroiodide | HCID 66704664 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178483720 | HCID 178483720 | 87.2% |
Reaction Steps
A solution of tert-butyl 3-(7-amino-2H-benzo[b][1,4]thiazin-4(3H)-yl)propyl(methyl)carbamate (0.52 g, 1.541 mmol) in dry ethanol (20 mL) was treated with methyl thiophene-2-carbimidothioate hydroiodide (0.879 g, 3.08 mmol) at room temperature and stirred over night (18 hours). The reaction was basified with saturated NaHCO3 solution (50 mL), and the product was extracted into CH2Cl2 (2×25 mL). The combined CH2Cl2 layers were washed with brine (20 mL) and dried (Na2SO4). The solvent was evaporated, and the crude material was purified by column chromatography (2:98 (2 M NH3 in MeOH):CH2Cl2) on silica gel to obtain the title product (0.60 g, 87%) as a solid. ESI-MS (m/z, %): 447 (MH+, 100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08106043B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-c842984bcf2048a7970d1df9eabcca63 |
| Source note | uspto-grants-2012_01 |