HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formaldehyde → HCID 68132266, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | HCID 68133610 | HCID 68133610 | — |
| Solvent | Formic Acid | HCID 284 | — |
| Product | HCID 68132266 | HCID 68132266 | — |
Reaction Steps
The free base released from 6.5 g. of rac.-4-(3,4-dichlorophenyl)-1,2,3,4-tetrahydro-6,7-dimethoxyisoquinoline hydrochloride is heated at 120°C. (bath temperature) for 1 hour with 10 ml. of formic acid and 10 ml. of 35% formalin solution. After evaporation, extraction with sodium carbonate solution and methylene chloride and acidification with ethanolic hydrogen chloride, there is obtained rac.-4-(3,4-dichlorophenyl)-1,2,3,4-tetrahydro-6,7-dimethoxy-2-methylisoquinoline hydrochloride which is recrystallized from methanol-ether and then melts at 243°-246°C. (softening at 238°C). The free base melts at 115°-116°C. after recrystallization from ether-petroleum ether.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03947456 |
| Source dataset | uspto-grants-1976_03 |
| ORD ID | ord-b6ee6435c8e048a5900a8909b59d16f0 |
| Source note | uspto-grants-1976_03 |