HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 66699138, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | HCID 66699126 | HCID 66699126 | — |
| Solvent | Thionyl Chloride | HCID 24386 | — |
| Product | HCID 66699138 | HCID 66699138 | 36% |
Reaction Steps
(4-Hydroxymethyl-pyrazol-1-yl)-acetic acid methyl ester (194 mg) was dissolved in 1,2-dichloroethane (2 mL) and thionylchloride (0.7 mL). The solution was refluxed for 2.5 hours. The reaction was cooled and concentrated in vacuo. The residue was poured into ice/water and basified with sat. Na2CO3 to pH 11. The aqueous phase was then extracted with ethyl acetate and the organic layer was washed with brine, dried over Na2SO4, filtered and the solvent was evaporated. The residue was purified by flash chromatography (silica gel, heptane:ethyl acetate=100:0 to 50:50) to give the title compound as a colorless oil (81 mg, 36%). MS (EI)=188.0 [M+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08138189B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-df027104f9e347108f2772a3753ef06b |
| Source note | uspto-grants-2012_03 |