In fact, as his mother died during childbirth, he was entrusted to Baya Ben Jaafar, a close relative of the family, to raise him.

Initially, Materi didn't succeed in getting a hospital internship because the protectorate authorities doubted his feelings regarding the French presence.

The reason behind this was Mahmoud's previous participation in nationalist gatherings with his older brothers, Ali and Hafiz, followers of Young Tunisians and former employees at Sadiki Hospital.

[citation needed] In March 1927, El Materi opened his own office in Bab Menara quarter, while continuing to work as a volunteering assistant at Sadiki Hospital.

During his stay in Dijon, Mahmoud El Materi wrote political articles in several newspapers including Le Populaire.

With Habib Bourguiba, El Materi belonged to the core of the founders of the Neo Destour (Ksar Hellal Congress of March 2, 1934), the ancestor of the Constitutional Democratic Rally, and he was chosen by his peers to become the first president of the party, a position he held for four years, until his resignation in 1938 following his organized strike in November the previous year.

With another brother, Tahar El Materi, Moncef established in the early 1970s a pharmaceutical firm called Al Adwya, one of Tunisia's biggest private drugs companies today.