HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 9976683, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 10424642 | HCID 10424642 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 9976683 | HCID 9976683 | — |
Reaction Steps
To the compound of Example 4, described above (79 mg, 0.26 mmol) in CH2Cl2 (0.5 mL) was added Et3N (72 uL, 0.52 mmol), and then methanesulfonyl chloride (25 uL, 0.31 mmol). The reaction exothermed to CH2Cl2 reflux briefly. The reaction was over within 1 min based on tlc (19:1 CH2Cl2/MeOH) and was poured into 10% NaOH (5 mL) and extracted with EtOAc (3×20 mL). The extracts were washed with H2O (10 mL) and satd aq Nacl (10 mL), dried (Na2SO4), concentrated and flash chromatographed (1×10 cm silica) with 0-8% MeOH in CH2Cl2 to afford 63 mg (65%). mp=186-187°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06222036B1 |
| Source dataset | uspto-grants-2001_04 |
| ORD ID | ord-72395c042bf04c8a954577364efd9520 |
| Source note | uspto-grants-2001_04 |