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6444234081
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3 (1 equiv), (DMF), -10°C to room temperature, 2 h, 38%; (b) pyridine (2.2 equiv), AcCl (1.1 equiv), DCM, 0°C then to room temperature, 2 h, AcCl (1.1 equiv), 0°C then to room temperature, 2 h, 71%. (10) Mp = 95-96°C. Stable at room temperature for over 4 months.
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6444222061
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note
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8 (12) Atomic coordinates for 1 and 6a are available upon request from the Cambridge Crystallographic Data Center, University Chemical Laboratory, Lensfield Road, Cambridge CB2 IEW (Deposition numbers: (1) CCDC 239364, (6a) CCDC 237660).
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