Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 67988083 | HCID 67988083 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178522293 | HCID 178522293 | — |
Reaction Steps
N-{1-[5-chloro-7-(phenylsulfonyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-4-piperidinyl}benzamide D41 (240 mg) and sodium methoxide (157 mg, 2.9 mmol) were dissolved in MeOH (15 ml). The reaction mixture was heated at 75° C. for 30 min and then extracted with EtOAc (150 ml); washed with water (60 ml), brine (2×60 ml). Yellow oil obtained, solvent removed to afford a yellow solid which was purified by prep HPLC (mobile phase: A: 0.01% NH4HCO3/H2O B; ACN. Column shimazu PRC-ODS 10.0 uM, 20×250 mm. Method 07.8 min 40-50% ACN 8-10 min 95˜95% ACN. Flow rate 30 mL/min to give product E44 as an ashen solid in 73 mg. LCMS [MH+] [email protected] min (5 min run)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09045485B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-1551c8d0260d4171958e3ba68092b76c |
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| Source note | uspto-grants-2015_06 |
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