HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 54429783, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1-Methyl-4-piperidone | HCID 74049 | — |
| Reactant | HCID 11020377 | HCID 11020377 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 54429783 | HCID 54429783 | 83% |
Reaction Steps
To a stirred solution of 4-azido-2,3,5,6-tetrafluorobenzaldehyde (23), 0.140 g, 0.640 mmol) and 1-methylpiperidine-4-one (0.040 mL, 0.32 mmol) in MeOH (1.5 mL), 1N aq. NaOH (0.650 mL, 0.650 mmol) was added dropwise. Yellow suspension resulted within minutes which was stirred at rt for forty-five minutes and diluted with water (3 mL). Yellow solid was collected by vacuum filtration, washed with water until the filtrate was neutral to pH paper. The yellow solid was dried further in vacuo to give 0.139 g (83%) 3,5-bis(4'-azido-2',3',5',6'-tetrafluorophenylmethylene)-1-methyl piperidine-4-one (22) as bright yellow powder; mp 153° C. (violent decomposition). 1HNMR(CDCL3 δ 2.37 (s, 3H), 3.42 (s, 4H), 7.55 (s,2H). ##STR28##
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06022597 |
| Source dataset | uspto-grants-2000_02 |
| ORD ID | ord-f83a8f8077a5475c9a614f92b75d4ab6 |
| Source note | uspto-grants-2000_02 |