Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 12333358 | HCID 12333358 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 15924245 | HCID 15924245 | — |
Reaction Steps
4.46 g (0.025 mol) of 4-methyl-5,6,7,8-tetrahydro- cumarin-5-one are dissolved in a mixture of 41.9 g of liquid methylamine in 100 ml of methanol pre- cooled to -9° C., With cooling, and heated to 180° C. for 3 hours in an autoclave. After cooling the methanol and methylamine are distilled off using a rotary evaporator, the residue is chromatographed on a silica gel column using ethylene chloride/ethanol (95:5) and recrystallised from cyclohexane/ethyl acetate (1:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05068334 |
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| Source dataset | uspto-grants-1991_11 |
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| ORD ID | ord-90b9317abe044c5780ff861c50340a73 |
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| Source note | uspto-grants-1991_11 |
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