Hydrochloric Acid → HCID 25111210、化合物

温度

0 °C

6.80 g (38 mmol) of 2-methyl-2-phenyl-propionic acid methyl ester was dissolved at rt in 200 mL MeCl2 and 7.01 ml (90.4 g=76 mmol) of dichloromethylmethylether was added and the mixture cooled down to 0° C.; 21.47 mL (36.93 g=191 mmol) TiCl4 was added over 15 min and the reaction warmed up to ambient temperature; stirring was continued for 16 hours. The reaction mixture was then treated at 0° C. with 20 ml of HCl (37% in water) and extracted twice with MeCl2; the organic phases were washed with water, dried over MgSO4, filtered and evaporated. The crude product was purified by chromatography (silicagel, eluent:gradient of n-heptane/EtOAc) to yield 5.00 g of the title compound as yellow oil. MS: 206.1 (M+).

1. temperaturethe reaction warmed up to ambient temperature
2. extractionextracted twice with MeCl2
3. washthe organic phases were washed with water
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. customevaporated
7. customThe crude product was purified by chromatography (silicagel, eluent:gradient of n-heptane/EtOAc)

ORDレコード

ord-5cc4fa502e1a4abf8341995c0ee1255f

出典データセット

uspto-grants-2010_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07772253B2