Perchloric Acid → O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine

HRID 44117

反応式

HRID 44117 の反応式
[C:1]1([CH3:19])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[S:9]([O:12][N:13]=C(OCC)C)(=[O:11])=[O:10].Cl(O)(=O)(=O)=O>O1CCOCC1>[C:1]1([CH3:19])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[S:9]([O:12][NH2:13])(=[O:11])=[O:10]

参加物

4

反応物 2

HCID 24247Perchloric AcidHCID 2724212Ethyl N-[[(2,4,6-trimethylphenyl)sulfonyl]oxy]ethanimidate

生成物 1

HCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
0 °C

実験手順

Ethyl N-mesitylsulfonyloxyacetimidate (20 g, 65.7 mmol, 1 eq) was dissolved in 1,4-dioxane (6 ml) and the solution was cooled to 0° C. To the mixture was added dropwise Perchloric acid (10 m), and the reaction mixture was then stirred at 0° C. for 45 minutes. The solution was poured into ice water, and the solid precipitated was filtered and washed with water and dried for 15 minutes in vacuum. The sample was stored in plastic container at −20° C. 1HNMR (400 MHz, DMSO-d6): δ 2.32 (s, 3H), 2.64 (s, 6H), 4.98 (br peak, 2H), 6.99 (s, 2H).

後処理

  1. customthe solid precipitated
  2. filtrationwas filtered
  3. washwashed with water
  4. customdried for 15 minutes in vacuum
  5. customwas stored in plastic container at −20° C

出典と根拠

ORDレコード
ord-31874d42e9e246259412665d9e168059
出典データセット
uspto-grants-2013_09
特許番号
US08536338B2

関連ノート

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