HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethyl phosphite → 2,3-Bis(diethoxyphosphoryl)-benzo[b]thiophene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethyl phosphite | HCID 31215 | — |
| Reactant | 2,3-Dibromo-1-benzothiophene | HCID 94977 | — |
| Catalyst | Palladium Chloride | HCID 24290 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2,3-Bis(diethoxyphosphoryl)-benzo[b]thiophene | HCID 87830000 | 60% |
Reaction Steps
A suspension of PdCl2 (0.15 g) in 2,3-dibromothianaphthene (2.4 g) was brought to the temperature of 115° C., and P(OEt)3 (3.3 g) was then dropped under stirring and in an inert atmosphere. Once dropping was completed, the red solution was brought to 160° C. After 1 h 30 min, the mixture was diluted with CH2Cl2, washed twice with water and dehydrated. The solvent was evaporated at reduced pressure to yield a residue that underwent chromatography on silica gel by flash chromatography (AcOEt), to yield 2,3-bis(diethoxyphosphoryl)-benzo[b]thiophene (1.6 g) (yield 60%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07307037B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-cbd6b1ef8bad466ca1449b9371fc67d1 |
| Source note | uspto-grants-2007_12 |