HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1,1-Dimethylethyl 2-bromo-4,5,7,8-tetrahydro-6H-thieno[2,3-d]azepine-6-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | tert-Butyl 4,5,7,8-tetrahydro-6H-thieno[2,3-d]azepine-6-carboxylate | HCID 57354994 | — |
| Solvent | Acetic acid chloroform | HCID 21584526 | — |
| Product | 1,1-Dimethylethyl 2-bromo-4,5,7,8-tetrahydro-6H-thieno[2,3-d]azepine-6-carboxylate | HCID 59302551 | — |
Reaction Steps
The product of step f) (10 mg, 0.039 mmol) dissolved in a 50:50 mixture of chloroform/acetic acid (1 ml) was treated with N-bromosuccinimide (7 mg, 0.041 mmol). The reaction mixture was stirred for 30 minutes at ambient temperature. The reaction mixture was poured into water (5 ml) and extracted with CHCl3 (3×5 ml). The combined organic phases were washed with 10% KOH solution (5 ml), brine (5 ml), dried (MgSO4), and concentrated to give the crude product as an oil. Purification by HPLC gave the subtitle compound as an oil. MS: ESI (positive): 332, 334 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07718647B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-6fd29d1d333f488b910518d67c8cf762 |
| Source note | uspto-grants-2010_05 |