HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 2-Methylpentane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 22258012 | HCID 22258012 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-Methylpentane | HCID 7892 | — |
| Product | HCID 22257992 | HCID 22257992 | — |
Reaction Steps
Methanesulfonyl chloride (0.028 ml) was added to a solution of 5-[(3-aminophenyl)thio]-3-methyl-1-(2-methylpropyl)-6-(1-naphthalenylmethyl) thieno[2,3-d]pyrimidine-2,4-(1H, 3H)-dione (60 mg) and triethylamine (0.067 ml) in anhydrous dichloromethane (2 ml) at room temperature. After 1 hour, saturated sodium hydrogen carbonate solution (10 ml) was added and the mixture was extracted with ether (2×10 ml). The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by preparative normal-phase HPLC with isohexane:ethyl acetate gradient elution then recrystallised from ethyl acetate:isohexane to give the title compound (28 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06180635B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-ae4e108403b64a1fadc5bec23141d697 |
| Source note | uspto-grants-2001_01 |