HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 137329926, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 137329923 | HCID 137329923 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 137329926 | HCID 137329926 | 66.1% |
Reaction Steps
AcCl (0.063 mL, 0.88 mmol) was added to a sol. of 2-[3-(tert-butyl-dimethyl-silanyloxymethyl)-4-chloro-phenyl]-ethylamine (252 mg, 0.840 mmol) and DIPEA (0.575 mL, 3.36 mmol) in CH2Cl2 (8.4 mL). The mixture was stirred at rt for 30 min, and aq. sat. NH4Cl was added. The layers were separated, and the org. layer was washed with aq. 1M NaOH, dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the crude by FC (CH2Cl2/MeOH 19:1) yielded the title compound (190 mg, 66%). LC-MS: tR=1.09 min; ES+: 342.19.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07799805B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-d73f5c921b674415a90c39d16910972d |
| Source note | uspto-grants-2010_09 |