HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloromethyl Methyl Ether → HCID 68284910, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloromethyl Methyl Ether | HCID 7864 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 178436240 | HCID 178436240 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68284910 | HCID 68284910 | 85.9% |
Reaction Steps
To a solution of 4-(2,6-diethyl-4-methylphenyl)-6-hydroxy-5-benzyloxy-2-methyl-3(2H)-pyridazinone (120 mg, 0.317 mmol) in dry DMF (2 ml) was added 60% sodium hydride (20 mg, 0.50 mmol) at 5° C. under nitrogen atmosphere. The mixture was stirred for 5 minutes, and then 80% chloromethyl methyl ether (0.04 ml, 0.47 mmol) was added. After ice-bath was removed, the mixture was stirred at room temperature for further 30 minutes. The reaction solution was diluted with water, and extracted with ethyl acetate 2 times. The combined organic layer was washed with water 2 times, washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give 115 mg of Compound (I-7-1) as oil (yield: 85%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029295B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-77144543fa11429086b6973ef903aebb |
| Source note | uspto-grants-2015_05 |