Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 2-Chloro-N,N-dimethylethylamine | HCID 7901 | — |
| Reactant | 4-hydroxy-5-methoxy-9H-fluoren-9-one | HCID 820269 | — |
| Reactant | N,N-Dimethylaminoethyl chloride hydrochloride | HCID 11636816 | — |
| Solvent | Chlorobenzene | HCID 7964 | — |
| Product | HCID 9862105 | HCID 9862105 | 91% |
Reaction Steps
In a manner similar to Example 2B, prepare the free base of 2 -chloroethyl-dimethylamine hydrochloride (0.60 g, 3.5 mmole). As before, separately prepare a solution of 4-hydroxy-5-methoxy-fluoren-9-one (0.54 g, 2.4 mmole) in methanol (4 mL) and chlorobenzene (12 mL), heating to 130° C. while stirring for 30 minutes. Cool reaction to 100° C. before adding the free base of 2-chloroethyl-dimethylamine prepared previously in 15 mL chlorobenzene. Proceed as before in Example 2B to obtain the title compound as an orange-yellow powder (0.79 g, 91%). m.p. 188-191° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06004959 |
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| Source dataset | uspto-grants-1999_12 |
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| ORD ID | ord-98efedee8ead417887d705d417541e94 |
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| Source note | uspto-grants-1999_12 |
|---|
