HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 4-(2,4-Dioxo-8-methyl-1,3,8-triazaspiro[4.5]-decan-3-yl)-2-(trifluoromethyl)-benzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 21846478 | HCID 21846478 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 4-(2,4-Dioxo-8-methyl-1,3,8-triazaspiro[4.5]-decan-3-yl)-2-(trifluoromethyl)-benzonitrile | HCID 21846487 | — |
Reaction Steps
Using the procedure of Example 2, 3 g of the product of Example 22, 70 ml of methanol and 17 ml of 2N hydrochloric were reacted and the solution was refluxed for 90 minutes. It was poured into 200 ml of ammonium hydroxide+100 g of ice saturated with sodium chloride and extraction was carried out 4 times with ethyl acetate. The extracts were washed with salt water, dried and purified on silica with methylene chloride-methanol: 9-1 as eluant. After crystallization from methylene chloride-isopropyl ether, 2.12 g of the expected product (white crystals) melting at 188°-189° C. were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05705654 |
| Source dataset | uspto-grants-1998_01 |
| ORD ID | ord-46beca51e86d4bf592c55a56f8a03990 |
| Source note | uspto-grants-1998_01 |