反应 #595316

反应方程式

thiobenzoic acid

Cs2CO3

→

cesium thiobenzoate

收率 83.4%

溶剂

methanol

反应条件

后处理

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

实验过程

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).

来源