HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron tribromide → HCID 59267961, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 59267860 | HCID 59267860 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59267961 | HCID 59267961 | 101.3% |
Reaction Steps
To a solution of 5-(2-benzyloxy-1,1-dimethyl-ethyl)-1,3,4-thiadiazol-2-ylamine (15.0 g, 57.0 mmol) in DCM (100 mL), boron tribromide (1N in DCM, 15.0 mL, 162.0 mmol) is added slowly at 0° C. The reaction mixture is warmed up to room temperature and stirred for 3 h. After cooling the reaction mixture to 0° C., ice water is added. The two phases are separated and the pH of the water phase is adjusted to ˜13 with NaOH and extracted with n-BuOH. The organic layer is washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to afford 10.0 g of 2-(5-amino-1,3,4-thiadiazol-2-yl)-2-methyl-propan-1-ol as a brown solid; m/z 174 [M+H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08362039B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-ed930ca8fdf14c62abe6672bc9f0e096 |
| Source note | uspto-grants-2013_01 |