تفاعل #595316

معادلة التفاعل

thiobenzoic acid

Cs2CO3

→

cesium thiobenzoate

المردود 83.4%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   workup.DISSOLUTIONwere dissolved
2. 2
   تركيزThe resulting solution was concentrated on the rotovap
3. 3
   workup.ADDITIONThe solid residue was diluted with 500 mL of acetone
4. 4
   ترشيحthe white solid (CsHCO3) was filtered off
5. 5
   أخرىwas removed
6. 6
   تركيزThe acetone was then concentrated

الإجراء التجريبي

To a solution of thiobenzoic acid (50.0 g, 361.8 mmol) in methanol (362 mL) was added Cs2CO3 (130 g, 398 mmol) in portions over 5 min. The resulting mixture was stirred 10 min until all solids were dissolved. The resulting solution was concentrated on the rotovap. The solid residue was diluted with 500 mL of acetone and the white solid (CsHCO3) was filtered off. This process was repeated two times to ensure all CsHCO3 was removed. The acetone was then concentrated to afford cesium thiobenzoate (Strijtveen, B.; Kellogg, R. M. J. Org. Chem. 1986, 51, 3664) as a yellow solid (81.5 g, 83%); 1H NMR (300 MHz, CD3OD) δ 7.25-7.38 (m, 3H), 8.09 (dd, J=1.4, 8.2 Hz, 2H).

المصدر