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Iodine → 3-(3-iodo-4-methoxybenzyl)-1H-1,2,4-triazole

HRID 1508549
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반응식

HRID 1508549 반응식
[CH3:1][O:2][C:3]1[CH:14]=[CH:13][C:6]([CH2:7][C:8]2[N:12]=[CH:11][NH:10][N:9]=2)=[CH:5][CH:4]=1.[I:15]I>CO.S([O-])([O-])(=O)=O.[Ag+2]>[I:15][C:14]1[CH:13]=[C:6]([CH:5]=[CH:4][C:3]=1[O:2][CH3:1])[CH2:7][C:8]1[N:12]=[CH:11][NH:10][N:9]=1
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참가 물질

5

반응물 2

HCID 807IodineHCID 178489902HCID 178489902, 화합물

생성물 1

HCID 1784899043-(3-iodo-4-methoxybenzyl)-1H-1,2,4-triazole

시약·촉매·용매 2

HCID 178418844HCID 178418844, 화합물촉매2회HCID 887Methanol용매

실험 절차

To a solution of 3-(4-methoxybenzyl)-1H-1,2,4-triazole (335 mg, 1.770 mmol) in MeOH (5 ml) under nitrogen at RT was added silver sulfate (552 mg, 1.770 mmol) followed by iodine (449 mg, 1.770 mmol). Added a second equivalent of silver sulfate and stirred for 3 days. The reaction did not go to completion. The solids were filtered washing with MeOH, the filtrate was concentrated, and the residue was purified by flash column chromatography on silica gel, eluting with MeOH in DCM to afford the title compound contaminated with ca. 20% of starting material. Mass spectrum (ESI) 316.1 (M+1).

후처리

  1. filtrationThe solids were filtered
  2. washwashing with MeOH
  3. concentrationthe filtrate was concentrated
  4. customthe residue was purified by flash column chromatography on silica gel
  5. washeluting with MeOH in DCM

출처 및 근거

ORD 기록
ord-cfaa3d88e7654d019e04623a8f363db9
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09221834B2

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