Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzylamine | HCID 7504 | — |
| Reactant | HCID 21833597 | HCID 21833597 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21833630 | HCID 21833630 | — |
Reaction Steps
A mixture of 8 g 8-(2-chloro-pyrimidin-4-yl)-1,4-dioxa-8-aza-spiro[4.5]decane 8a) and 7.2 ml benzylamine is heated for 2 hours at 150° C., then cooled, admixed with 20 ml water and the aqueous solution is extracted three times with 20 ml methylene chloride each time. After drying the combined organic phases over sodium sulfate and removing the solvent, the residue is washed with cold isohexane. In this way 9.6 g benzyl-[4-(1,4-dioxa-8-aza-spiro[4.5]dec-8-yl)-pyrimidin-2-yl]amine is obtained as a yellow powder. 1H-NMR (d6 -DMSO): δ=7.85 ppm (d, 1H); 7.40-7.18 (m, 5H) 7.15 (broad s, 1H, NH); 6.12 (d, 1H); 4.45 (d, 2H); 3.96 (s, 4H); 3.65 (m, 4H); 1.61 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05972947 |
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| Source dataset | uspto-grants-1999_10 |
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| ORD ID | ord-a39b2eb14da845cd9b143e7950ef6451 |
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| Source note | uspto-grants-1999_10 |
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