Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86621185 | HCID 86621185 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 903579-36-2 | HCID 11578126 | 90.1% |
Reaction Steps
A sol. of compound 10 (13.8 g, 16.9 mmol) in CH2Cl2 (120 mL) was cooled to 0° C. HCl (4M in dioxane, 120 mL) was added. The mixture was stirred for 1 h at 0° C., then 2 h at rt. The solvents were removed under reduced pressure, and the residue was dried under high vacuum. The residue was diluted with CH2Cl2, and washed with aq. 1M NaOH until the aq. layer staid basic. The org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (MeOH/CH2Cl2 5:95→10:90→20:80 with 1% Et3N all the time) yielded the title compound (9.45 g, 90%). LC-MS: tR=0.87 min; ES+: 620.40.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07915259B2 |
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| Source dataset | uspto-grants-2011_03 |
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| ORD ID | ord-42cf549915cb4e73b633530918ae5d4a |
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| Source note | uspto-grants-2011_03 |
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