Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 67236887 | HCID 67236887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86649121 | HCID 86649121 | 100% |
Reaction Steps
The product from Example 191B (3.14 g, 7.84 mmole) was dissolved in 70 mL CH2Cl2 and cooled in an ice-acetone bath to −10° C. Triethylamine (3.82 mL, 27.4 mmole) was added dropwise to the cold solution, followed by dropwise addition of methanesulfonyl chloride (1.53 mL, 19.59 mmole) in 20 mL CH2Cl2 over 10 minutes. The resulting clear solution was stirred in the cold for 90 min. The reaction was deemed complete by LC-MS analysis and the solvent was removed in vacuo leaving a light yellow solid as the title compound, (4.36 g, 100%), that was used directly in the next reaction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09006387B2 |
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| Source dataset | uspto-grants-2015_04 |
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| ORD ID | ord-9de170311ce94d35ba8280017c8e81af |
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| Source note | uspto-grants-2015_04 |
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