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Bis(trifluoroacetoxy)iodobenzene → HCID 57831017, 화합물

HRID 240318
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HRID 240318 반응식
[C:1]([C:3]1[N:4]=[C:5]2[C:18](=NO)[C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[C:6]2=[N:7][C:8]=1[C:9]([NH2:11])=[O:10])#[N:2].FC(F)(F)C(OI(C1C=CC=CC=1)OC(=O)C(F)(F)F)=[O:24]>CC#N.O>[C:1]([C:3]1[N:4]=[C:5]2[C:18](=[O:24])[C:17]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[C:6]2=[N:7][C:8]=1[C:9]([NH2:11])=[O:10])#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 102317Bis(trifluoroacetoxy)iodobenzeneHCID 178510554HCID 178510554, 화합물

생성물 1

HCID 57831017HCID 57831017, 화합물수율 58%

시약·촉매·용매 1

HCID 18373917Acetonitrile--water (1/1)용매

실험 절차

A suspension of 33 (522 mg, 1.97 mmol) and [bis(trifluoroacetoxy)iodo]benzene (1.69 g, 3.9 mmol) in CH3CN/H2O (9:1, 20 ml) was stirred 24 h at room temperature. The solid was collected by filtration and washed with CH3CN. The residue was dissolved in DMSO (2 ml) and precipitated by addition of H2O. The obtained solid was filtered and dried under vacuum, affording 36 (286 mg, 58%) as light brown solid. 1H NMR (300 MHz, DMSO d6): δ 8.65 (bs, 1H), 8.31 (bs, 1H), 8.09 (dd, 1H), 7.93 (m, 2H), 7.77 (ddd, 1H). ESI+MS: calcd for C13H6N4O2: 250.22; found: 251.1 (MH+).

후처리

  1. filtrationThe solid was collected by filtration
  2. washwashed with CH3CN
  3. dissolutionThe residue was dissolved in DMSO (2 ml)
  4. customprecipitated by addition of H2O
  5. filtrationThe obtained solid was filtered
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-5e1a7a796765490dbb757b7ddc31d46d
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08648076B2

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