Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 11559966 | HCID 11559966 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11590678 | HCID 11590678 | — |
Reaction Steps
To a stirred solution of the compound from example 1 (100 mg, 0.26 mmol) in dichloromethane (3 mL) was added triethylamine (54.4 μL, 0.39 mmol) at room temperature. The solution was cooled to 0° C. and methanesulfonyl chloride (24 μl, 0.31 mmol) was added. The reaction was stirred for a further 45 minutes. The reaction mixture was then diluted with water (5 mL) and stirred vigorously for 5 minutes. The phases were separated and the organic phase concentrated in vacuo to give the crude residue which was azeotroped with ethyl acetate to afford the product as a crystalline solid, 78 mg (65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07456170B2 |
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| Source dataset | uspto-grants-2008_11 |
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| ORD ID | ord-fae6532fc7a9418aa46ae9ee5a76414e |
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| Source note | uspto-grants-2008_11 |
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