P-Toluenesulfonamide → N-tosyliminophenyliodinane

HRID 252222

反応式

HRID 252222 の反応式
C(O[C:5]1[C:6](OC(=O)C)=[C:7]([I:11])[CH:8]=[CH:9][CH:10]=1)(=O)C.[OH-].[K+].[CH3:18][C:19]1[CH:20]=[CH:21][C:22]([S:25]([NH2:28])(=[O:27])=[O:26])=[CH:23][CH:24]=1>CO>[C:19]1([CH3:18])[CH:20]=[CH:21][C:22]([S:25]([N:28]=[C:7]2[CH2:6][CH2:5][CH2:10][CH2:9][I:11]2[C:7]2[CH:6]=[CH:5][CH:10]=[CH:9][CH:8]=2)(=[O:27])=[O:26])=[CH:23][CH:24]=1

参加物

5

反応物 3

HCID 6269P-ToluenesulfonamideHCID 14797Potassium HydroxideHCID 21865429Bis(acetoxy)iodobenzene

生成物 1

HCID 86611515N-tosyliminophenyliodinane収率 113.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Diacetoxyiodobenzene (12.88 g, 40 mmol) was added to a solution of KOH (5.61 g, 100 mmol) and p-toluenesulfonamide (6.85 g, 40 mmol) in methanol (160 mL) at 8° C. A yellow color developed within 1 minute. The cooling bath was removed, and the solution was allowed to warm to RT with stirring for 3 hours. Water (180 mL) was added and the reaction was refrigerated overnight. The precipitate was collected by filtration and dried overnight in a vacuum dessicator to yield 10 g (66%) of a light yellow solid which was used with out further purification or characterization.

後処理

  1. customThe cooling bath was removed
  2. additionWater (180 mL) was added
  3. waitthe reaction was refrigerated overnight
  4. filtrationThe precipitate was collected by filtration
  5. customdried overnight in a vacuum dessicator

出典と根拠

ORDレコード
ord-d3bd792dcf0f4539a355ce4befb7d585
出典データセット
uspto-grants-2011_01
特許番号
US07868023B2

関連ノート

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