2-Methylbenzoxazole → 2-Methyl-1,3-benzoxazole-6-sulfonyl chloride

HRID 409700

反応式

HRID 409700 の反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].[CH3:6][C:7]1[O:8][C:9]2[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=2[N:11]=1>>[CH3:6][C:7]1[O:8][C:9]2[CH:15]=[C:14]([S:2]([Cl:1])(=[O:5])=[O:3])[CH:13]=[CH:12][C:10]=2[N:11]=1

参加物

3

反応物 2

HCID 72252-MethylbenzoxazoleHCID 24638Chlorosulfonic acid

生成物 1

HCID 545939422-Methyl-1,3-benzoxazole-6-sulfonyl chloride収率 59.9%

反応条件

温度
117.5 °C

実験手順

Chlorosulfonic acid (12.5 ml, 187.8 mmol) was cooled in an ice bath and 2-methylbenzoxazole (5.0 g, 37.5 mmol) was carefully added drop wise over a period of 15 min. The combined mixture was heated at 115-120° C. for 16 hours. After cooling, the mixture was added very slowly to ca. 100 ml ice/water mix. The white solid that separated was collected by filtration, washed with water until washings were neutral and dried to yield 5.2 g (59%) of Compound 8, whose structure is given below:

後処理

  1. customof 15 min
  2. temperatureAfter cooling
  3. additionmix
  4. customThe white solid that separated
  5. filtrationwas collected by filtration
  6. washwashed with water until washings
  7. customdried

出典と根拠

ORDレコード
ord-19cba7e21bd745dd95faab713c599489
出典データセット
uspto-grants-2014_06
特許番号
US08759526B2

関連ノート

読み込み中…