Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | HCID 14624217 | HCID 14624217 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 14624180 | HCID 14624180 | — |
Reaction Steps
A solution of 2 g (5.37 mmol) of N-{3-[(methyl)(3,4-dimethoxyphenethyl)amino]propyl}salicylamide in 18 ml of chloroform and 1 ml of acetic acid is treated for 2 min with a stream of gaseous hydrochloric acid. 340 milligrams of trioxymethylene are then added to the above mixture, which is heated for 20 min to 70°-75° C. After return to room temperature, a stream of nitrogen is passed through for 30 min and the mixture is then filtered on a sinter and evaporated to dryness. The residue is taken up in toluene and re-evaporated to dryness in a rotary evaporator under vacuum. The solid residue (3.10 g) is ground in isopropyl ether and filtered. The cream powder obtained (m=2.1 g) is recrystallized in a 75:25 i-PrOH/EtOH mixture to give 1.53 g (yld=68%) of compound A of formula: ##STR6##
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05071850 |
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| Source dataset | uspto-grants-1991_12 |
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| ORD ID | ord-efaea55f22e6469eada7fef9dae6f354 |
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| Source note | uspto-grants-1991_12 |
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