Water → 2,4-Dichloro-5-methylpyridine

HRID 1992648노트

반응식

HRID 1992648 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([CH2:9]Cl)=[CH:4][N:3]=1.C(N(CC)CC)C.O>C(O)C.[Ni].CCOC(C)=O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([CH3:9])=[CH:4][N:3]=1

참가 물질

7

반응물 3

HCID 962WaterHCID 8471TriethylamineHCID 27627282,4-Dichloro-5-(chloromethyl)pyridine

생성물 1

HCID 126437182,4-Dichloro-5-methylpyridine

시약·촉매·용매 3

HCID 935Nickel촉매HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

2,4-Dichloro-5-chloromethyl-pyridine (1.43 g, 7.28 mmol) is dissolved in ethanol (14 ml). After addition of triethyl amine (737 mg, 7.28 mmol), Raney nickel (143 mg) is added. The reaction vessel is connected to a balloon filled with H2. After 3 hours of very vigorous magnetically stirring at RT, NMR analysis of a reaction aliquot indicated complete conversion of the starting material. The reaction mixture is diluted with EtOAc and poured into water.

후처리

  1. additionis added
  2. additionfilled with H2
  3. customNMR analysis of a reaction aliquot indicated complete conversion of the starting material

출처 및 근거

ORD 기록
ord-79a391b269bb465b85cdd312f2bedf29
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07648989B2

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