HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chlorobenzaldehyde → HCID 59235218, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chlorobenzaldehyde | HCID 7726 | — |
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | HCID 13617480 | HCID 13617480 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59235218 | HCID 59235218 | 101.8% |
Reaction Steps
998 mg of methyl 2-amino-2-(4-methoxyphenyl)acetate (prepared according to M. A. Sierra Rodrigez et al, Int. Pat. Appl. WO 02/102762) are dissolved in 30 mL of dichloromethane. 1 g of magnesium sulphate is added along with 717 mg of 4-chlorobenzaldehyde. The mixture is stirred at AT for 21 hours, the solid is filtered off, the filtrate is washed with dichloromethane then the solvent is dried over magnesium sulphate and evaporated to produce 1.65 g of an oil. The crude product is purified by chromatography over silica gel while eluting with the 90/10/1 then 80/20/1 heptane/ethyl acetate/triethylamine mixture. 1.24 g of colourless oil is obtained which crystallises on cooling (Yd=76%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08168667B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-b3363a23f69248a7899a350babe5410a |
| Source note | uspto-grants-2012_05 |