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Ethyl orthoformate → HCID 57851246, 화합물

HRID 77755
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HRID 77755 반응식
[I:1][C:2]1[CH:3]=[C:4]([NH3+:16])[CH:5]=[C:6]([C:8](=[O:15])[NH:9][CH:10]([CH3:14])[CH2:11][O:12][CH3:13])[CH:7]=1.[N-:17]=[N+:18]=[N-:19].[Na+].[CH:21](OCC)(OCC)OCC>CC(O)=O>[I:1][C:2]1[CH:7]=[C:6]([CH:5]=[C:4]([N:16]2[CH:21]=[N:19][N:18]=[N:17]2)[CH:3]=1)[C:8]([NH:9][CH:10]([CH3:14])[CH2:11][O:12][CH3:13])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 31214Ethyl orthoformateHCID 33557Sodium AzideHCID 866173873-Iodo-5-(2-methoxy-1-methyl-ethylcarbamoyl)-phenyl-ammonium

생성물 1

HCID 57851246HCID 57851246, 화합물수율 72.6%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of 3-Iodo-5-(2-methoxy-1-methyl-ethylcarbamoyl)-phenyl-ammonium (7.47 g, 22.4 mmol) and NaN3 (2.68 g, 41.2 mmol) in AcOH (100 mL) was added HC(OEt)3 (18.3 mL, 110 mmol) at room temperature. The reaction mixture was brought to reflux for 4 hours, then cooled to room temperature. The solvent was removed in vacuo and the residue was purified by silica-gel chromatography to give 3-Iodo-N-(2-methoxy-1-methyl-ethyl)-5-tetrazol-1-yl-benzamide as a white solid (6.30 g, 72%). MS (M+H)=388.

후처리

  1. temperatureto reflux for 4 hours
  2. customThe solvent was removed in vacuo
  3. customthe residue was purified by silica-gel chromatography

출처 및 근거

ORD 기록
ord-a8d9f366adda4904abd2b9dde9ac86eb
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841336B2

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