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Triethylamine → 4-Ethylamino-5-nitro-2-phenylpyrimidine

HRID 842062
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인쇄 미리보기

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HRID 842062 반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][N:5]=[C:4]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:3]=1.Cl.[CH2:18]([NH2:20])[CH3:19].C(N(CC)CC)C>C(O)(C)C>[CH2:18]([NH:20][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][N:5]=[C:4]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:3]=1)[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 11198Ethylamine hydrochlorideHCID 22617793HCID 22617793, 화합물

생성물 1

HCID 226177974-Ethylamino-5-nitro-2-phenylpyrimidine수율 93.3%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 4-chloro-5-nitro-2-phenylpyrimidine (3 g), ethylamine hydrochloride (1.6 g), triethylamine (3.9 g) and isopropanol (60 ml) is refluxed for three hours. The reaction mixture is concentrated under reduced pressure, and to the residue are added chloroform and water. The chloroform layer is separated, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (eluent; chloroform), and recrystallized from isopropanol to give the desired compound (2.9 g).

후처리

  1. temperatureis refluxed for three hours
  2. concentrationThe reaction mixture is concentrated under reduced pressure
  3. additionto the residue are added chloroform and water
  4. customThe chloroform layer is separated
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue is purified by silica gel column chromatography (eluent; chloroform)
  8. customrecrystallized from isopropanol

출처 및 근거

ORD 기록
ord-857f86fbe7524e19a8d3afb9365d8686
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06372740B1

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