[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[C:8]([Br:10])[CH:7]=[C:6]([NH2:11])[CH:5]=1.CCN(CC)CC.[Cl:20][CH2:21][CH2:22][CH2:23][C:24](Cl)=[O:25]>C(Cl)Cl.CCOC(C)=O>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:5]=[C:6]([NH:11][C:24](=[O:25])[CH2:23][CH2:22][CH2:21][Cl:20])[CH:7]=[C:8]([Br:10])[CH:9]=1
To a solution of 3-amino-5-bromo-benzoic acid methyl ester (D12) (460 mg, 2.0 mmol, 1 equiv) in CH2Cl2 (10 ml) at room temperature was added NEt3 (306 μl, 2.2 mmol, 1.1 equiv) then 4-chlorobutyrylchloride (247 μl, 2.2 mmol, 1.1 equiv). The resulting mixture was stirred at room temperature for 16 h and then diluted with AcOEt. The organic phase was washed with 2N aqueous HCl solution, dried over MgSO4 and concentrated in vacuo to give 3-bromo-5-(4-chloro-butanoylamino)-benzoic acid methyl ester (D13) (530 mg, 79%) as a pale yellow oil. RT=2.88 s
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