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Ethyl Acetate → 4,6-Dichloro-2-ethylpyrimidin-5-amine

HRID 345425
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HRID 345425 반응식
[Cl:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([Cl:11])[N:5]=[C:4]([CH2:12][CH3:13])[N:3]=1.CCOC(C)=O>CO.[Ni]>[NH2:8][C:7]1[C:2]([Cl:1])=[N:3][C:4]([CH2:12][CH3:13])=[N:5][C:6]=1[Cl:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8857Ethyl AcetateHCID 2306474,6-Dichloro-2-ethyl-5-nitropyrimidine

생성물 1

HCID 5220474,6-Dichloro-2-ethylpyrimidin-5-amine수율 100%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

4,6-Dichloro-5-nitro-2-ethylpyrimidine (185 g, 0.83 mol) was dissolved in methanol (1.5 L) and reduced under 15 p.s.i. H2 in the presence of Raney nickel (30 g) for 5 hr. The mixture was filtered through Celite (washing well with MeOH) and the filtrate was evaporated to dryness to give 159.1 g (0.83 mol, quantitative yield) of the title compound as a chromatographically pure (silica gel plates, developed with EtOAc:hexanes, 3:1) dark liquid which was used directly in the next step.

후처리

  1. filtrationThe mixture was filtered through Celite (
  2. washwashing well with MeOH) and the filtrate
  3. customwas evaporated to dryness

출처 및 근거

ORD 기록
ord-2d015bf70a38492d953c1045a0440294
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05057517

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