Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 67315886 | HCID 67315886 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 67314829 | HCID 67314829 | — |
Reaction Steps
118.4 g (259 mmol, 1.0 equivalent) of {[4-(benzylidene)aminomethylbenzyl]-(4-dipropylaminobutyl)amino}ethyl acetate (8a) and 900 ml of ethanol were charged in a 3-liter four-necked flask and cooled to 0° C. The mixture was added dropwise with 870 ml (2.59 mol, 10 equivalents) of 3N hydrochloric acid over 2.5 hours and stirred at 0° C. for one hour and at 25° C. for 18 hours. About 5% of the raw material (8a) remained as a result of confirmation by HPLC. Therefore, the reaction solution was added with 110 ml of 2N hydrochloric acid at 25° C. After three hours, the content of the raw material (8a) was measured by HPLC, and it was confirmed that the content decreased to 1% or less.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07977512B2 |
|---|
| Source dataset | uspto-grants-2011_07 |
|---|
| ORD ID | ord-489ded5bb3f54487ac808c40e64776f2 |
|---|
| Source note | uspto-grants-2011_07 |
|---|