HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 67596032, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | N,N-Dimethylaminoethyl chloride hydrochloride | HCID 11636816 | — |
| Reactant | HCID 15858911 | HCID 15858911 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 67596032 | HCID 67596032 | 59% |
Reaction Steps
To a solution of Compound 88 (1.0 g, 1.98 mmol) obtained in Example 88 in 10 ml of N,N-dimethylformamide was portionwise added sodium hydride (60% in oil, 166 mg, 4.15 mmol) with stirring at room temperature, and 2-dimethylaminoethylchloride hydrochloride (298 mg, 2.07 mmol) was added thereto, followed by heating to 80° C. and then stirring for one hour. A saturated aqueous solution of ammonium chloride was added to the reaction solution for neutralization, water was added thereto, and the resulting crystals were collected by filtration to give 1.1 g of a crude product. The obtained crude product was recrystallized from ethanol (65 ml) to give 0.67 g (yield: 59%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05891902 |
| Source dataset | uspto-grants-1999_04 |
| ORD ID | ord-978bb373ba5f480ab38ea80f15044d1d |
| Source note | uspto-grants-1999_04 |