Benzyl Chloride → N-benzyl-thiazolinethion

温度

150 °C

12.7 g (0.1 mole) of benzylchloride were added to 209.2 g (1 mole) of 2-benzylthio-thiazoline and the mixture was heated to 150° C. for eight hours. The mixture was allowed to cool down to 70° C. and 500 ml of methanol were added. The reaction mixture was allowed to cool down to room temperature and stirred for an additional hour; N-benzyl-thiazoline-thion precipitated from the medium as a white crystalline product, was isolated by filtration and washed twice with 10 ml of methanol. The crude product was recrystallized from a minimum of acetonitrile. 146 g of N-benzyl-thiazolinethion were isolated and sulfonated as described below.

1. temperatureto cool down to 70° C.
2. temperatureto cool down to room temperature
3. customN-benzyl-thiazoline-thion precipitated from the medium as a white crystalline product
4. customwas isolated by filtration
5. washwashed twice with 10 ml of methanol
6. customThe crude product was recrystallized from a minimum of acetonitrile

ORDレコード

ord-789ad516cc7a459dbf3e7dacc4f95292

出典データセット

uspto-grants-2004_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06733947B2