HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → 6,7-Bis(3-hydroxyphenyl)-pteridin-4-ylamine methanesulfonate salt
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 3-[4-Amino-7-(3-hydroxyphenyl)pteridin-6-yl]phenol | HCID 10088066 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 6,7-Bis(3-hydroxyphenyl)-pteridin-4-ylamine methanesulfonate salt | HCID 86594138 | 97.11% |
Reaction Steps
1.308 g (13.63 mmol) of methanesulfonic acid in 10 mL of MeOH was added to the suspension of 2.15 g (6.48 mmol) of 6,7-bis(3-hydroxyphenyl)-pteridin-4-ylamine in 10 mL of MeOH. The mixture became homogeneous and orange-red in color. It was stirred for 30 min and then added dropwise to 400 mL of diethyl ether with vigorous stirring. The formed yellow precipitate was collected, washed with diethyl ether and dried in vacuo to give 2.69 g (97.11% yield) of the product as a light-yellow powder. Mass-spec [ES+]=332.8. 1H NMR (MeOH-d4) 2.70 (3H, s), 6.86–6.90 (2H, m), 6.99–7.01 (2H, m), 7.04–7.08 (2H, m), 7.16–7.21 (2H, m), 8.80 (1H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07208493B2 |
| Source dataset | uspto-grants-2007_04 |
| ORD ID | ord-00ca0ef48ae6460abf535c4db1d89927 |
| Source note | uspto-grants-2007_04 |