Dichloromethane → HCID 17764601, compound

To a stirred solution of 2,5-dichloro-3-methylthiophene [prepared according to the method of J. Amer. Chim. Soc., 1971, 333.] (11.8 g) in CH2Cl2 (200 mL) was added TiCl4(37.94 g) and dichloromethyl methyl ether (12.6 g) at −10° C. After stirring for 4 hours, the reaction mixture was poured into ice-water and the whole was stirred vigorously for 30 minutes. The resulting mixture was extracted with CH2Cl2 (200 ml×1), and the organic layers was washed with saturated NaHCO3 solution(100 mL×1), brine (100 mL×1), dried over MgSO4, and concentrated in vacuo. The resulting residue was purified by distillation (bp: 140-145° C./10 mmHg) to provide the subtitle compound (11.75 g).

1. stirringthe whole was stirred vigorously for 30 minutes
2. extractionThe resulting mixture was extracted with CH2Cl2 (200 ml×1)
3. washthe organic layers was washed with saturated NaHCO3 solution(100 mL×1), brine (100 mL×1)
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. distillationThe resulting residue was purified by distillation (bp: 140-145° C./10 mmHg)

ORD record

ord-0129fc2a09e44cd0b01f620e7a67df42

Source dataset

uspto-grants-2004_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06696470B2