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N-(hydroxymethyl)phthalimide → HCID 53328541, 화합물

HRID 1190873
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HRID 1190873 반응식
O[CH2:2][N:3]1[C:7](=[O:8])[C:6]2=[CH:9][CH:10]=[CH:11][CH:12]=[C:5]2[C:4]1=[O:13].[Br:14][C:15]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:16]=1[CH3:24]>OS(C(F)(F)F)(=O)=O>[Br:14][C:15]1[C:16]([CH3:24])=[CH:17][C:18]([N+:21]([O-:23])=[O:22])=[CH:19][C:20]=1[CH2:2][N:3]1[C:7](=[O:8])[C:6]2[C:5](=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:4]1=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8354N-(hydroxymethyl)phthalimideHCID 2516721-Bromo-2-methyl-4-nitrobenzene

생성물 1

HCID 53328541HCID 53328541, 화합물수율 94.4%

시약·촉매·용매 1

HCID 62406Trifluoromethanesulfonic acid용매

실험 절차

N-(Hydroxymethyl)phtalimide (2.36 g, 13.3 mmol) was dissolved in 20 mL of triflic acid at 0° C. The mixture was stirred for 20 minutes and then 2-bromo-5-nitrotoluene (2.88 g, 1 eq) was added. This solution was allowed to warm to room temperature and was stirred for 18 h. The mixture was poured slowly into 300 mL of ice-cold water. The aqueous layer was extracted with DCM. The combined organic layers were washed with 100 mL of water, dried over Na2SO4, filtered and evaporated to yield expected compound as a white solid (4.71 g, 94% yield).

후처리

  1. stirringwas stirred for 18 h
  2. extractionThe aqueous layer was extracted with DCM
  3. washThe combined organic layers were washed with 100 mL of water
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-16257a32f1734483b23335fe4c3f7518
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680095B2

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