HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → 9-ethyl-9H-carbazole-3,6-dicarbaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | N-ethyl carbazole | HCID 6836 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Product | 9-ethyl-9H-carbazole-3,6-dicarbaldehyde | HCID 3716675 | 40% |
Reaction Steps
109 g of DMF was cooled down to 0° C., and 228 g of phosphorous oxychloride was slowly dropped therein. The resultant was heated up to room temperature, and then 30 g of N-ethylcarbazole and 75 ml of 1,2-dichloroethane were dropped therein. The reaction of the mixture was carried out at 90° C. for 20 hours, thereafter the solution was cooled down to room temperature. The solution was poured into 1.5 l of ice water, and extracted with chloroform, dried with anhydrous MgSO4, and was separated with hexane and ethyl acetate in a column. The reaction yield was about 40%. The structure analysis was confirmed by 1H-NMR, which was shown in FIG. 6.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06124046 |
| Source dataset | uspto-grants-2000_09 |
| ORD ID | ord-3986f67dc9174634841918f7a8a49b19 |
| Source note | uspto-grants-2000_09 |