تفاعل #71070

معادلة التفاعل

amino-thioxo-acetic acid ethyl ester

1,3-dichloro-propan-2-one

EtOAc

N2

→

title compound

4-Chloromethyl-thiazole-2-carboxylic acid ethyl ester

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux
2. 2
   غسيلthe mixture was washed with sat. aq. NaHCO3 (10 mL)
3. 3
   تجفيفThe organic layer was dried over MgSO4
4. 4
   ترشيحfiltered
5. 5
   أخرىthe solvent removed under reduced pressure
6. 6
   أخرىPurification of the residue by FC (4:1 hept-EA)

الإجراء التجريبي

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a mixture of amino-thioxo-acetic acid ethyl ester (2.50 g, 18.77 mmol) and 1,3-dichloro-propan-2-one (2.88 g, 21.59 mmol) in toluene (20.0 mL) was stirred for 2 h at reflux. EtOAc (20 mL) was added at rt and the mixture was washed with sat. aq. NaHCO3 (10 mL) followed by brine (20 mL). The organic layer was dried over MgSO4, filtered, and the solvent removed under reduced pressure. Purification of the residue by FC (4:1 hept-EA) gave the title compound as a light yellow oil. TLC:rf (4:1 hept-EA)=0.26. LC-MS-conditions 02: tR=0.89 min, [M+H]+=206.40.

المصدر