Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86676047 | HCID 86676047 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59469955 | HCID 59469955 | 69% |
Reaction Steps
The obtained 9-acetyl-3,6-bis(triphenylsilyl)carbazole (1.97 g) was dissolved in tetrahydrofuran (50 mL). A 50% by mass aqueous sodium hydroxide solution (1.1 g) was added to the solution. The resultant mixture was stirred at 50° C. for 3 hours and cooled to room temperature. Diluted hydrochloric acid was added thereto until the pH reached 5, followed by stirring for 30 min. The mixture was extracted with methylene chloride. The separated organic layer was washed with water and dried, and the methylene chloride was evaporated. The residue was purified with a recycle HPLC (name of apparatus: Recycling Preparative HPLC LC-9201, product of Japan Analytical Industry Co., Ltd., developing solvent: THF, flow rate: 3.5 mL/min), to thereby obtain 1.28 g of 3,6-bis(triphenylsilyl)carbazole as colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09206202B2 |
|---|
| Source dataset | uspto-grants-2015_12 |
|---|
| ORD ID | ord-86413646ef934f639cf9627e456002ef |
|---|
| Source note | uspto-grants-2015_12 |
|---|