Methanesulfonyl chloride → Methyl 2-[(methanesulfonyl)oxy]-4-nitrobenzoate

HRID 280833

反応式

HRID 280833 の反応式
[OH:1][C:2]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH3:15][S:16](Cl)(=[O:18])=[O:17]>C(Cl)(Cl)Cl.C(N(CC)CC)C>[CH3:15][S:16]([O:1][C:2]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5])(=[O:18])=[O:17]

参加物

5

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 139539Salicylic acid, 4-nitro-, methyl ester

生成物 1

HCID 23320160Methyl 2-[(methanesulfonyl)oxy]-4-nitrobenzoate

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8471Triethylamine溶媒

反応条件

温度
50 °C

実験手順

Methyl 2-hydroxy-4-nitrobenzoate (19.7 g) was dissolved in 100 ml of chloroform and triethylamine (15 ml). The solution was kept at a temperature below 15° C., and methanesulfonylchloride (8.6 ml) was added dropwise. The solution was maintained at 50° C. for 1 hr, whereupon it was poured onto ice-hydrochloric acid and extracted with a total of 600 ml chloroform. The solution was dried with magnesium sulfate, treated with active carbon and evaporated. The product was recrystallized from methanol. Yield: 20 g.

後処理

  1. additionwas added dropwise
  2. additionwas poured onto ice-hydrochloric acid
  3. extractionextracted with a total of 600 ml chloroform
  4. dry with materialThe solution was dried with magnesium sulfate
  5. additiontreated with active carbon
  6. customevaporated
  7. customThe product was recrystallized from methanol

出典と根拠

ORDレコード
ord-e999d4d5001244278c3eb477e6871205
出典データセット
uspto-grants-1986_05
特許番号
US04591584

関連ノート

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