HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 10200034, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 10200885 | HCID 10200885 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10200034 | HCID 10200034 | 24% |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
[2-Methoxy-4-(3-methyl-pyrazol-1-yl)-phenyl](5H,11H-pyrrolo[2,1-c][1,4]-benzodiazepin-10-yl) methanone (0.82 g) from Example 107 was dissolved in dichloromethane (20 ml) and cooled to −78° C. Boron tribromide (6.2 ml) was added and the reaction stirred at 0° C. for five minutes. Ammonium hydroxide (15 ml) was added and extracted with dichloromethane. The organic phase was washed with brine and dried over anhydrous magnesium sulfate. The solid was removed by filtration and the solvent removed in vacuo. The residue was purified by flash column chromatography on silica pressure eluting with hexane/ethyl acetate (3/1 then 2/1) to afford 0.19 g of the title compound as a colorless solid, m.p. 134-136° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06511974B1 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-77a4fcd287e3471091f23d65fee15711 |
| Source note | uspto-grants-2003_01 |