Water → 2,4-Dichloro-5-methylpyridine

HRID 1992648ノート

反応式

HRID 1992648 の反応式
[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

参加物

7

反応物 3

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

生成物 1

HCID 126437182,4-Dichloro-5-methylpyridine

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-79a391b269bb465b85cdd312f2bedf29
出典データセット
uspto-grants-2010_01
特許番号
US07648989B2

反応ノート

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