Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 13119197 | HCID 13119197 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 67650750 | HCID 67650750 | 99.3% |
Reaction Steps
A 0° C. solution of 4.5 g of product from Example 333 in 77.8 ml of diethyl ether and 25.5 ml of water is treated with 2.58 g of solid sodium bicarbonate followed by 7.6 g of iodine. The reaction is stirred for 3 hours at 0° C. then at room temperature overnight. The mixture is cooled to 0° C. and sodium sulfite is added until the reaction is colorless. The solution is extracted with diethyl ether, dried and concentrated in vacuo to give 7.0 g of an oil. The oil is purified by chromatography (Silica gel: 5% diethyl ether/hexane) to give 2.8 g of Isomer A and 1.86 g of Isomer B. Isomer A:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05744465 |
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| Source dataset | uspto-grants-1998_04 |
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| ORD ID | ord-92b33441fd90496a8ba46800a6d6c5be |
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| Source note | uspto-grants-1998_04 |
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