HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 44243000, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 57908084 | HCID 57908084 | — |
| Reactant | HCID 57908095 | HCID 57908095 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 44243000 | HCID 44243000 | — |
Reaction Steps
Solutions each of 2B (1.0 equivalent), 2-(3-ethylureido)benzo[b]thiophene-3-carboxylic acid (2C, 1.25 equivalents), DMF (0.14 M), EDC (1.25 equivalents), and HOBT (1.25 equivalents) is added triethylamine (1.0 equivalent) at room temperature. After stirring for 12 hr, the reaction is complete as determined by LCMS analysis. The reaction mixture is then partitioned between ethyl acetate and water and the separated organics is dried over Na2SO4, filtered, and concentrated under reduced pressure. Purification by preparatory LCMS provides N-((8-(2-(3-ethylureido)benzo[b]thiophene-3-carbonyl)-4-oxo-1,3,8-triazaspiro[4.5]dec-1-en-2-yl)methyl)acetamide (2), respectively.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07981904B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-f4bbe372a6714cfdac95ca23bce6d63e |
| Source note | uspto-grants-2011_07 |