Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Calciumoxide | HCID 6850728 | — |
| Reactant | 4-(4-Bromobutoxy)-1,2-dichlorobenzene | HCID 18768634 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18176647 | HCID 18176647 | 80.6% |
Reaction Steps
A mixture of 4-(4-bromobutoxy)- 1,2-dichlorobenzene (0.03 mol), methylamine (20 g) and calciumoxide (7 g) in THF (100 ml) was stirred at 125° C. overnight in an autoclave. The mixture was filtered over dicalite and the filtrate was evaporated. The residue was taken up in DIPE and the mixture was filtered over dicalite. The filtrate was converted into the hydrochloric acid salt (1:1) with HCl/2-propanol. The precipitate was filtered off and dried, yielding 6 g (70.3%) of 4-(3,4-dichlorophenoxy)-N-methyl-1-butanamine (intermediate 4, mp. 132° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06602873B2 |
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| Source dataset | uspto-grants-2003_08 |
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| ORD ID | ord-7d09998466384c6996cf8fb9602ffc90 |
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| Source note | uspto-grants-2003_08 |
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