Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 23598693 | HCID 23598693 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69601283 | HCID 69601283 | — |
Reaction Steps
A solution of {6-hydroxymethyl-3-[(isoquinoline-1-carbonyl)-amino]-2-oxo-2,3,4,7-tetrahydro-azepin-1-yl}-acetic acid methyl ester, 19, (1.35 g, 3.52 mmol) in 10 mL CH2Cl2is treated with triethyl amine (1.3 mL, 8.81 mmol) and methanesulfonyl chloride (0.61 mL, 7.93 mmol) at −78° C. After stirring at −78° C. for 2 hours, the reaction mixture is poured into a CH2Cl2/saturated NaCl solution. The organic layer is collected and washed with saturated NaHCO3, saturated NaCl, dried (Na2SO4) and concentrated in vacuo to afford the desired product which is used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07001899B2 |
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| Source dataset | uspto-grants-2006_02 |
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| ORD ID | ord-756d1c4ce3f94e9ba4a7fb136739bb55 |
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| Source note | uspto-grants-2006_02 |
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