반응 #595316

반응 방정식

thiobenzoic acid

Cs2CO3

→

cesium thiobenzoate

수율 83.4%

용매

methanol

반응 조건

후처리

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

실험 절차

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).

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