Methanol → Methyl 3-(5-methyl-1,2,4-oxadiazol-3-YL)benzoate

HRID 330794ノート

反応式

HRID 330794 の反応式
S(=O)(=O)(O)O.[CH3:6][C:7]1[O:11][N:10]=[C:9]([C:12]2[CH:13]=[C:14]([CH:18]=[CH:19][CH:20]=2)[C:15]([OH:17])=[O:16])[N:8]=1.O.[CH3:22]O>>[CH3:6][C:7]1[O:11][N:10]=[C:9]([C:12]2[CH:13]=[C:14]([CH:18]=[CH:19][CH:20]=2)[C:15]([O:17][CH3:22])=[O:16])[N:8]=1

参加物

5

反応物 4

HCID 887MethanolHCID 962WaterHCID 1118Sulfuric AcidHCID 71278183-(5-Methyl-1,2,4-oxadiazol-3-yl)benzoic acid

生成物 1

HCID 53429639Methyl 3-(5-methyl-1,2,4-oxadiazol-3-YL)benzoate

実験手順

7.83 ml (147 mmol) of concentrated sulfuric acid are added to a suspension of 30.0 g (147 mmol) of 3-(5-methyl-1,2,4-oxadiazol-3-yl)benzoic acid in 150 ml of methanol, and the mixture is heated at the boil for 18 hours. The reaction mixture is cooled in an ice bath, water is added, the mixture is filtered off with suction and washed well with water: methyl 3-(5-methyl-1,2,4-oxadiazol-3-yl)benzoate as colourless crystals; m.p. 81° C., ESI 219 (M+H), HPLC: Rt.=2.65 min (method A).

後処理

  1. temperaturethe mixture is heated at the boil for 18 hours
  2. temperatureThe reaction mixture is cooled in an ice bath
  3. filtrationthe mixture is filtered off with suction
  4. washwashed well with water
  5. custom=2.65 min (method A)

出典と根拠

ORDレコード
ord-9e97ec0013794d7495789bd38f7c513f
出典データセット
uspto-grants-2014_11
特許番号
US08877751B2

反応ノート

読み込み中…