The general procedure for the synthesis of 3-chloro-2,2-dichloromethylpropan-1-ol from pentaerythritol was as follows: pentaerythritol (15 g, 0.11 mol) was dissolved in pyridine (27 ml) and heated to 65 °C. Thionyl chloride (24.7 ml, 0.33 mol) was added slowly and dropwise over a period of 4 h. The temperature of the reaction was controlled to be between 65°C and 95°C. After completion of the reaction, the reaction mixture was continued to be stirred at 50 °C for 18 hours. Subsequently, the reaction solution was heated to 120 °C-130 °C for concentration and then cooled to room temperature. The concentrated reaction solution was slowly poured into ice water (75 ml) and stirred for 30 minutes. The resulting solid product was collected by filtration, washed well with water and dried to give 3-chloro-2,2-bis(chloromethyl)propan-1-ol (15.4 g, 73% yield).
[1] Patent: KR101592370, 2016, B1. Location in patent: Paragraph 0204; 0205; 0206; 0207
[2] Australian Journal of Chemistry, 1988, vol. 41, # 12, p. 1953 - 1962
[3] Patent: US2835709, 1955,
[4] Mededelingen van de Koninklijke Vlaamse Academie voor Wetenschappen, Letteren en Schone Kunsten van Belgie, Klasse der Wetenschappen, 1940, vol. 2, # 5, p. 3,16
