4-Fluorobenzoic Acid → 3-(Chlorosulfonyl)-4-fluorobenzoic acid

HRID 33781

反応式

HRID 33781 の反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][CH:8]=1>>[Cl:1][S:2]([C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][C:7]=1[F:6])[C:11]([OH:13])=[O:12])(=[O:5])=[O:3]

参加物

3

反応物 2

HCID 99734-Fluorobenzoic AcidHCID 24638Chlorosulfonic acid

生成物 1

HCID 39298913-(Chlorosulfonyl)-4-fluorobenzoic acid

反応条件

温度
150 °C

実験手順

Chlorosulphonic acid (100 ml, 1.5 mol) was gradually added to 4-fluorobenzoic acid (43 g, 0.307 mol) with stirring. The clear dark yellow mixture was heated to 150° C. for 24 hours. The yellow solution was cooled back to room temperature and poured onto ice with vigorous stirring. The white precipitate was filtered and pressed dry. The solid was dried overnight in a desiccator under vacuum and over activated silica (54.65 g, 75%). Mp: 116-117° C.; m/z (LC-MS, ESP), RT=4.03 min, (M−−1)=237-239 (ratio 1:3).

後処理

  1. temperatureThe yellow solution was cooled back to room temperature
  2. additionpoured onto ice with vigorous stirring
  3. filtrationThe white precipitate was filtered
  4. custompressed dry
  5. customThe solid was dried overnight in a desiccator under vacuum and over activated silica (54.65 g, 75%)

出典と根拠

ORDレコード
ord-b5bb2f4675124571b48d8ac00275062e
出典データセット
uspto-grants-2008_09
特許番号
US07429660B2

関連ノート

読み込み中…