Chlorosulfonic acid → 2-Oxazol-5-YL-benzenesulfonyl chloride

HRID 29522ノート

反応式

HRID 29522 の反応式
[C:1]1([C:7]2[O:11][CH:10]=[N:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:12][S:13](O)(=[O:15])=[O:14]>C(Cl)(Cl)Cl>[O:11]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][C:6]=2[S:13]([Cl:12])(=[O:15])=[O:14])=[CH:8][N:9]=[CH:10]1

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 5893115-Phenyl oxazole

生成物 1

HCID 552794732-Oxazol-5-YL-benzenesulfonyl chloride

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
70 °C

実験手順

5-Phenyloxazole (2.0 g, mmol) in chloroform (50 ml) was cooled to 0° C. using an ice bath. Chlorosulfonic acid 4.8 g (2.7 ml, 3 eq) of was added slowly with stirring. The reaction mixture was heated to 70° C. for 16 h. The reaction mixture was then cooled to RT, quenched with ice and extracted with chloroform. The organic layer was washed with cold water, brine and concentrated. The brown solid obtained was purified by column chromatography using 5% ethyl acetate in pet ether as eluent, to yield a yellow solid.

後処理

  1. temperatureThe reaction mixture was then cooled to RT
  2. customquenched with ice
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with cold water, brine
  5. concentrationconcentrated
  6. customThe brown solid obtained
  7. customwas purified by column chromatography
  8. customto yield a yellow solid

出典と根拠

ORDレコード
ord-77ee1a4a12604140807a12e2e1e125b3
出典データセット
uspto-grants-2008_09
特許番号
US07420055B2

反応ノート

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