HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 68949993, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 68948880 | HCID 68948880 | — |
| Product | HCID 68949993 | HCID 68949993 | 34% |
Reaction Steps
Add sodium tetrahydroborate (0.36 g, 9.52 mmol) in portions to a solution of (4-bromo-phenyl)-(1-methyl-azetidin-3-yl)-methanone (0.64 g, 2.38 mmol) in CH2Cl2 at 0° C. Stir the mixture at RT overnight and quench with water. Adjust the aqueous to pH=10 by using 1 N NaOH and extract with ethylacetate (2×150 mL). Dry the combined organic layers over Na2SO4, filter, and concentrate. Purify the crude material by flash chromatography, collecting all the fractions as the product does not show by UV. Elute with 10% MeOH (2 N NH3)/CH2Cl2 to give 0.22 g (34%) of the title compound. LC-MS/ES m/z (79Br) 270.0 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08263772B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-1abbd5b64e974bfebd1c172efb562e96 |
| Source note | uspto-grants-2012_09 |