Water → HCID 70081578、化合物

HRID 461339ノート

反応式

HRID 461339 の反応式
[CH2:1]([N:3]([CH2:6]C)CC)[CH3:2].[CH2:8]([C:15]1[C:20]([NH2:21])=CC=CN=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.Cl[CH2:23][C:24]([Cl:26])=O.[OH2:27]>C1C=CC=CC=1>[CH2:8]([CH2:15][C:20]([NH:21][C:6]1[C:24]([Cl:26])=[CH:23][CH:2]=[CH:1][N:3]=1)=[O:27])[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

6

反応物 4

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 189526852-Benzylpyridin-3-amine

生成物 1

HCID 70081578HCID 70081578、化合物収率 92%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒3 回

実験手順

3.4 ml tri-ethylamine is added to a solution of 4.5 g (0.025 mol) 2-benzyl-3-aminopyridine in 25 ml dry benzene. A solution of 2 ml chloro-acetyl chloride in 40 ml dry benzene is then added with stirring to this solution at a temperature of 5°-10° C. The mixture is stirred for 30 minutes at room temperature and a precipitate forms. This precipitate is redissolved by addition of 50 ml water and 50 ml benzene to the mixture. The organic phase is subsequently separated off, dried, and evaporated to dryness. The residue, a white solid, is recrystallized from a little benzene, giving 5.78 g (92%) 2-benzyl-3-chloro-acetamidopyridine of melting point 145°-147° C.

後処理

  1. stirringThe mixture is stirred for 30 minutes at room temperature
  2. customThe organic phase is subsequently separated off
  3. customdried
  4. customevaporated to dryness
  5. customThe residue, a white solid, is recrystallized from a little benzene

出典と根拠

ORDレコード
ord-a1c92ce32d7b47cfb539f427963d5278
出典データセット
uspto-grants-1977_12
特許番号
US04062848

反応ノート

読み込み中…