تفاعل #69926

معادلة التفاعل

2-Bromothiophene-3-carboxylic acid

MeOH

SOCl2

→

2-bromothiophene-3-carboxylic acid methyl ester

ظروف التفاعل

المعالجة

1. 1
   أخرىthe mixture was degassed
2. 2
   أخرىpurged with nitrogen (2×)
3. 3
   تركيزThe mixture was then concentrated
4. 4
   workup.ADDITIONDCM (150 mL) was added
5. 5
   workup.ADDITIONSaturated NaHCO3 (20 mL) was added
6. 6
   workup.STIRRINGthe resulting mixture was stirred at room temperature for 15 minutes
7. 7
   غسيلThe organic layer was washed with saturated NaHCO3 (20 mL), water (20 mL), and saturated aqueous NaCl (20 mL)
8. 8
   تجفيفdried over Na2SO4
9. 9
   ترشيحfiltered
10. 10
    تركيزconcentrated

الإجراء التجريبي

2-Bromothiophene-3-carboxylic acid (5.0 g, 24 mmol, 1 eq.) was dissolved in MeOH (100 mL) and the mixture was degassed and purged with nitrogen (2×). SOCl2 (15 mL, 0.2 mol, 8.3 eq.) was added dropwise and the resulting mixture was stirred for two days at room temperature. The mixture was then concentrated and DCM (150 mL) was added. Saturated NaHCO3 (20 mL) was added, and the resulting mixture was stirred at room temperature for 15 minutes. The organic layer was washed with saturated NaHCO3 (20 mL), water (20 mL), and saturated aqueous NaCl (20 mL), then dried over Na2SO4, filtered and concentrated to yield 2-bromothiophene-3-carboxylic acid methyl ester (5.1 g) as a yellow oil.

المصدر