Methanesulfonyl chloride → N-(3-ethynylphenyl)methanesulfonamide

HRID 38225

反応式

HRID 38225 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:7]=[CH:8][CH:9]=1)[NH2:6])#[CH:2].[CH3:10][S:11](Cl)(=[O:13])=[O:12]>N1C=CC=CC=1>[C:1]([C:3]1[CH:4]=[C:5]([NH:6][S:11]([CH3:10])(=[O:13])=[O:12])[CH:7]=[CH:8][CH:9]=1)#[CH:2]

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 104682Benzenamine, 3-ethynyl-

生成物 1

HCID 57131399N-(3-ethynylphenyl)methanesulfonamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 3-ethynyl aniline (1.05 mL, 10.0 mmol) in pyridine (5 mL) was added methanesulfonyl chloride (857 μL, 1.10 eq.) at a temperature of 0° C. The resulting mixture was stirred overnight at room temperature and was then evaporated. The residue was treated with 2 N aq. HCl (25 mL) and subsequently extracted with ethyl acetate (2×30 mL). The combined organic layers were dried over MgSO4 and evaporated to give the desired methanesulfonamide in quantitative yield. It was used without further purification.

後処理

  1. customwas then evaporated
  2. additionThe residue was treated with 2 N aq. HCl (25 mL)
  3. extractionsubsequently extracted with ethyl acetate (2×30 mL)
  4. dry with materialThe combined organic layers were dried over MgSO4
  5. customevaporated

出典と根拠

ORDレコード
ord-e04eb91ca7634a4a97f9b40e63bc61d3
出典データセット
uspto-grants-2013_09
特許番号
US08524724B2

関連ノート

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