Chloroform → 2,4-Difluoro-5-methylbenzenesulfonyl chloride

HRID 46401

反応式

HRID 46401 の反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[F:6][C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[CH3:14].C(Cl)(Cl)Cl>>[F:13][C:11]1[CH:12]=[C:7]([F:6])[C:8]([CH3:14])=[CH:9][C:10]=1[S:2]([Cl:1])(=[O:5])=[O:3]

参加物

4

反応物 3

HCID 6212ChloroformHCID 24638Chlorosulfonic acid2 回HCID 679832,4-Difluoro-1-methylbenzene

生成物 1

HCID 594365302,4-Difluoro-5-methylbenzenesulfonyl chloride収率 75.1%

実験手順

Chlorosulfonic acid (5.2 mL, 0.078 mol) was added dropwise to a solution of 2,4-difluorotoluene (4.00 g, 0.0312 mol) in chloroform (75 mL, 0.94 mol). The reaction was stirred 2 hours. Additional chlorosulfonic acid (3.1 mL, 0.047 mol) was added and stirring was continued for 18 hours. The reaction was evaporated to an oil and poured onto ice. The mixture was extracted two times with ethyl ether. The combined organic phase was dried over magnesium sulfate and treated with activated carbon. The mixture was filtered through diatomaceous earth and the filtrate was evaporated to give 5.31 g of light brown oil.

後処理

  1. stirringstirring
  2. waitwas continued for 18 hours
  3. customThe reaction was evaporated to an oil
  4. additionpoured onto ice
  5. extractionThe mixture was extracted two times with ethyl ether
  6. dry with materialThe combined organic phase was dried over magnesium sulfate
  7. additiontreated with activated carbon
  8. filtrationThe mixture was filtered through diatomaceous earth
  9. customthe filtrate was evaporated

出典と根拠

ORDレコード
ord-6a7202be207d4465aeb64585adedb843
出典データセット
uspto-grants-2013_09
特許番号
US08541588B2

関連ノート

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