Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | HCID 10927507 | HCID 10927507 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18432370 | HCID 18432370 | — |
Reaction Steps
0.5 g (1.25 mmol) of 1-chloro-2-(8-chloro-4,4-dimethyl-1,1-dioxothiochroman-7-yl)carbonylcyclohex-1-en-3-one was dissolved in 10 ml of tetrahydrofuran, and 0.13 g (1.37 mmol) of N,O-dimethylhydroxylamine hydrochloride and 0.28 g (2.74 mmol) of triethylamine were added dropwise. The mixture was stirred at 25° C. for 25 hours, stirred into water and extracted with ethyl acetate, the organic phases were extracted with 1N hydrochloric acid and dried and the solvent was removed. This gave 0.4 g of beige crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06440899B1 |
|---|
| Source dataset | uspto-grants-2002_08 |
|---|
| ORD ID | ord-983b614ae5af43979b3f844d2eae4874 |
|---|
| Source note | uspto-grants-2002_08 |
|---|
