2-Bromomethylnaphthalene → HCID 936893、化合物

HRID 1033002ノート

反応式

HRID 1033002 の反応式
N[C:2]1[C:3](SC(C)(C)C)=[N:4][C:5](C)=[C:6](CC)[CH:7]=1.BrC[C:18]1[CH:27]=[CH:26][C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=1.[CH:28]([N:31](C(C)C)CC)(C)C>C(#N)C>[C:21]1([CH2:28][NH:31][C:3]2[CH:2]=[CH:7][CH:6]=[CH:5][N:4]=2)[C:20]2[C:25](=[CH:26][CH:27]=[CH:18][CH:19]=2)[CH:24]=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 703202-BromomethylnaphthaleneHCID 81531DiisopropylethylamineHCID 10105052HCID 10105052、化合物

生成物 1

HCID 936893HCID 936893、化合物収率 62.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 3-amino-2-tert-butylthio-5-ethyl-6-methylpyridine (0.15 g, 0.67 mmol), 2-bromomethyl-napthalene (0.15 g, 0.67 mmol), diisopropylethylamine (86 mg, 0.67 mmol) in acetonitrile (5 mL) was refluxed under an atmosphere of nitrogen for 16 hours. The resultant mixture was concentrated under reduced pressure (15 (torr). The residue was subjected to column chromatography on silica gel (50, elution with 1% methanol in chloroform). Collection and concentration of appropriate fractions provided 98 mg (40%) of the napthylmethylaminopyridine.

後処理

  1. temperaturewas refluxed under an atmosphere of nitrogen for 16 hours
  2. concentrationThe resultant mixture was concentrated under reduced pressure (15 (torr)
  3. customCollection and concentration of appropriate fractions

出典と根拠

ORDレコード
ord-8809eb84f1ad4137842a7d6249b0298f
出典データセット
uspto-grants-1994_05
特許番号
US05308854

反応ノート

読み込み中…