Dichloroacetyl chloride → 2,2-Dichloro-N-(2-ethynylphenyl)Acetamide

2-Ethynylaniline (1.0 g, 8.53 mmol) was dissolved in anhydrous dichloromethane (20 mL) with triethylamine (1.6 mL, 11.0 mmol). The mixture was cooled in an ice-bath under nitrogen, then a solution of dichloroacetyl chloride (0.875 mL, 8.53 mmol) in anhydrous dichloromethane (20 mL) was added dropwise. After the addition was completed the ice-bath was removed and the mixture was stirred at room temperature for 2 h. The reaction mixture was then washed successively with water, 10% hydrochloric acid and saturated sodium bicarbonate solution. The organic solution was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to give the title compound as a beige solid.

1. temperatureThe mixture was cooled in an ice-bath under nitrogen
2. additionAfter the addition
3. customwas removed
4. washThe reaction mixture was then washed successively with water, 10% hydrochloric acid and saturated sodium bicarbonate solution
5. dry with materialThe organic solution was dried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure

ORDレコード

ord-9c92edf1de184c30a73fd1a7c6b7fe55

出典データセット

uspto-grants-2008_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07326790B2