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

HRID 44117

반응식

HRID 44117 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-31874d42e9e246259412665d9e168059
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536338B2

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