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p-Toluidine → 2,6-Bis(p-tolylamino)-3-nitro-pyrimidine

HRID 2353574
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인쇄 미리보기

반응식

HRID 2353574 반응식
Cl[CH:2]1[N:7]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:5][C:4](Cl)=[N:3]1.[CH3:12][C:13]1[CH:14]=[CH:15][C:16]([NH2:19])=[CH:17][CH:18]=1.CC[N:22]([CH:26]([CH3:28])[CH3:27])C(C)C>O1CCOCC1>[C:13]1([CH3:12])[CH:18]=[CH:17][C:16]([NH:19][CH:2]2[N:7]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:5][C:4]([NH:22][C:26]3[CH:27]=[CH:18][C:13]([CH3:14])=[CH:12][CH:28]=3)=[N:3]2)=[CH:15][CH:14]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7813p-ToluidineHCID 81531DiisopropylethylamineHCID 184699722,6-Dichloro-3-nitropyrimidine

생성물 1

HCID 670914402,6-Bis(p-tolylamino)-3-nitro-pyrimidine수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
200 °C

실험 절차

A mixture of 2,6-dichloro-3-nitropyrimidine (194 mg, 1 mmol), p-tolylamine (236 mg, 2.2 mmol) and DIEA (524 μL, 3 mmol) in 3 mL dioxane was stirred in microwave at 200° C. for 20 min. After removal of the solvent, the residue was dissolved in chloroform and subjected to silica gel column purification to give 319 mg (yield: 95%) title compound. Calculated mass=335. Observed mass=336.

후처리

  1. customAfter removal of the solvent
  2. dissolutionthe residue was dissolved in chloroform
  3. customsubjected to silica gel column purification

출처 및 근거

ORD 기록
ord-76a9c0c08d764b68abb7491848b0a17f
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07749999B2

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