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HCID 19979377, 화합물 → 6-Chloro-2,4-bis(1-methylethyl)-3-pyridinamine

HRID 1461766
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HRID 1461766 반응식
[Cl:1][C:2]1[N:7]=[C:6]([CH:8]([CH3:10])[CH3:9])[C:5]([N+:11]([O-])=O)=[C:4]([CH:14]([CH3:16])[CH3:15])[CH:3]=1.[H][H]>O1CCCC1.[Ni]>[Cl:1][C:2]1[N:7]=[C:6]([CH:8]([CH3:9])[CH3:10])[C:5]([NH2:11])=[C:4]([CH:14]([CH3:16])[CH3:15])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 19979377HCID 19979377, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 199793736-Chloro-2,4-bis(1-methylethyl)-3-pyridinamine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 8028Tetrahydrofuran용매

실험 절차

30.0 g of 6-chloro-2,4-diisopropyl-3-nitropyridine are dissolved in 450 ml of tetrahydrofuran and, after the addition of 30.0 g of Raney nickel (suspended in ethanol), hydrogenated under a hydrogen pressure of 20 bar at from +30° C. to +35° C. The reaction mixture is filtered over diatomaceous earth and the filtrate is concentrated. The residue is purified by column chromatography on silica gel (eluant: ethyl acetate/hexane 3). 6-Chloro-2,4-diisopropyl-3-aminopyridine is obtained in the form of a clear crystalline powder, m.p. 53°-56° C.

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후처리

  1. customat from +30° C. to +35° C
  2. filtrationThe reaction mixture is filtered over diatomaceous earth
  3. concentrationthe filtrate is concentrated
  4. customThe residue is purified by column chromatography on silica gel (eluant: ethyl acetate/hexane 3)

출처 및 근거

ORD 기록
ord-cdb7e2cb074443f4b345d32e6dc614cc
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05077304

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