HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → 3-(4-Bromophenyl)propyl methanesulphonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-(4-Bromophenyl)propan-1-ol | HCID 10560614 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-(4-Bromophenyl)propyl methanesulphonate | HCID 19688466 | 98.9% |
Reaction Steps
To a stirred solution of 3-(4-Bromophenyl)propan-1-ol (500 g, 2.30 mol) and diisopropylethylamine (312 g, 2.40 mol) in anhydrous dichloromethane (4 L) at 0˜5° C. was added dropwise methanesulphonyl chloride (280 g, 2.40 mol) slowly. After addition, the reaction mixture was stirred for 1 hour at 0˜5° C. The reaction mixture was washed with brine (1 L) twice. The organic phase was concentrated in vacuo to afford the subtitle compound (i) (667 g). HPLC Retention Time=1.353 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08198285B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-1f92c5e26ddd484ea11e7af9ea1e0168 |
| Source note | uspto-grants-2012_06 |