Cesium carbonate → Cesium thiobenzoate

HRID 508134ノート

反応式

HRID 508134 の反応式
[C:1]([OH:9])(=[S:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C([O-])([O-])=O.[Cs+:14].[Cs+]>CO>[C:1]([O-:9])(=[S:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cs+:14]

参加物

4

反応物 2

HCID 10796Cesium carbonateHCID 178526132HCID 178526132、化合物

生成物 1

HCID 23707493Cesium thiobenzoate収率 83.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  1. dissolutionwere dissolved
  2. concentrationThe resulting solution was concentrated on the rotovap
  3. additionThe solid residue was diluted with 500 mL of acetone
  4. filtrationthe white solid (CsHCO3) was filtered off
  5. customwas removed
  6. concentrationThe acetone was then concentrated

出典と根拠

ORDレコード
ord-85526bdd15824d929ca1206a744dae88
出典データセット
uspto-grants-2015_08
特許番号
US09095565B2

反応ノート

読み込み中…