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

HRID 33781

반응식

HRID 33781 반응식
[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]

참가 물질

3

반응물 2

HCID 99734-Fluorobenzoic AcidHCID 24638Chlorosulfonic acid

생성물 1

HCID 39298913-(Chlorosulfonyl)-4-fluorobenzoic acid

반응 조건

온도
150 °C

실험 절차

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).

후처리

  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%)

출처 및 근거

ORD 기록
ord-b5bb2f4675124571b48d8ac00275062e
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429660B2

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