*3.3. Preparation of NOTA-PODS-ZEGFR:03115 and NODA-PODS-ZEGFR:03115*

In a 1.5 mL low-protein-binding centrifuge tube, a freshly prepared solution of TCEP-HCl in 1 M phosphate buffer pH 7 (0.025 mg/μL, 9.8 μL, 1.71 μmol) was added to a solution of ZEGFR:03115-Cys (200 μL, 2.3 mg/mL, 68.4 nmol). The mixture was incubated in a thermo shaker at 85 ◦C for 5 min (900 rpm) followed by 25 min at room temperature. Either NOTA-PODS or NODAGA-PODS solution in DMF was then added (1.03 μmol) and the solution was incubated in a thermo shaker at 37 ◦C for 1 h (900 rpm). The reaction mixture was analyzed by RP–HPLC. The product was purified by semi-preparative RP–HPLC. The collected fractions containing the product were dried and quantified by measuring the UV absorbance at 280 nm.

NOTA-PODS-ZEGFR:03115 = yield 38.5%. Analytical RP–HPLC (Gradient 2): Rt: 11:06 min:sec; ESI–HRMS (*m*/*z*): [M + H]<sup>+</sup> expected: 7470, found: 7470.91.

NODAGA-PODS-ZEGFR:03115 = yield 39.9%. Analytical RP–HPLC (Gradient 2): Rt: 11:08 min:sec; ESI–HRMS (*m*/*z*): [M + H]<sup>+</sup> expected: 7543, found: 7543.07.
