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Fragment couplings and cyclizations to the target molecule α‐Amanitin (1): a) MSA, COMU, DIPEA, DMA, 0 °C to r.t. 3 h; b) (a and b: onepot), H‐Asn‐Hyp‐OFm⋅HCl (4), HATU, DIPEA, DMF, 0 °C to r.t., 2 h; c) Et2NH, DMF, 1 h, r.t.; d) 1 m TBAF, THF, r.t., 2 h, 77 % over four steps; e) HATU, DIPEA, DMF, r.t., 16 h, 68 %, f) BF3⋅OEt2, EtSH, r.t., 2 h; g) mCPBA, iPrOH/EtOH (2:1), r.t., 30 min, 35 % over two steps.
