The present invention relates to a new process for the preparation of (3R)-3-fluoropyrrolidine hydrochloride or an acceptable salts thereof via a N-Boc-(3S)-3-hydroxypyrrolidine intermediate. The process is suitable for the synthesis of N-Boc-(3S)-3-hydroxypyrrolidine at technical scale in high, not less than 99.85%-a/a optical purity and a purity of not less than 99.8%-a/a. The high quality N-Boc-(3S)-3-hydroxypyrrolidine can be converted to (3R)-3-fluoropyrrolidine hydrochloride exhibiting an optical purity of not less than 99.95%-a/a and a purity of not less than 99.5%-a/a thus making it a suitable intermediate for manufacturing of pharmaceutical active compounds.