HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 87901234, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | HCID 87901224 | HCID 87901224 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 87901234 | HCID 87901234 | — |
Reaction Steps
A solution of Example 8D (4.54 g, 26.7 mmol), N,O-dimethyl hydroxylamine hydrochloride (5.6 g, 57 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (5.19 g, 27 mmol), 1-hydroxybenzotriazole (4.12 g, 30.5 mmol), and N-methylmorpholine (7.0 mL, 64 mmol) in dichloromethane (270 mL) at room temperature was stirred for 4 hours, diluted with dichloromethane, washed sequentially with aqueous NaHCO3, brine, 10% KHSO4, and brine, dried (MgSO4), filtered, and concentrated. Flash column chromatography (silica gel, 10% ethyl acetate/hexanes) provided the desired product. MS (ESI(+)) m/e 214 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07030262B2 |
| Source dataset | uspto-grants-2006_04 |
| ORD ID | ord-2c6d89360b9742f088bdd9f6d7a9b235 |
| Source note | uspto-grants-2006_04 |