Ammonia → 4-(4-Methylthiophenoxy)benzylamine

HRID 1591109ノート

反応式

HRID 1591109 の反応式
[NH3:1].[CH3:2][C:3]1[CH:17]=[CH:16][C:6]([S:7][C:8]2[CH:15]=[CH:14][C:11]([CH2:12]Br)=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.O>CO>[CH3:2][C:3]1[CH:17]=[CH:16][C:6]([S:7][C:8]2[CH:15]=[CH:14][C:11]([CH2:12][NH2:1])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 962WaterHCID 1317178844-(4-Methylthiophenoxy)benzylbromide

生成物 1

HCID 435288314-(4-Methylthiophenoxy)benzylamine収率 53%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a stirred mixture of 28% aq NH3 (40 ml) and methanol (200 ml) was added dropwise a solution (20 ml) of 4-(4-methylthiophenoxy)benzylbromide (5.00 g, 16.2 mM) in methanol at room temperature, and the mixture was stirred for 4 days at the same temperature. To the mixture was added water (100 ml), and the mixture was concentrated in vacuo. The residue was diluted with chloroform, and the mixture was washed with water and brine, dried with sodium sulfate, and concentrated in vacuo. The residue was chromatographed over alumina to give 4-(4-methylthiophenoxy)benzylamine (2.11 g, 53%) as colorless crystals, m.p. 61.8° C.

後処理

  1. concentrationthe mixture was concentrated in vacuo
  2. additionThe residue was diluted with chloroform
  3. washthe mixture was washed with water and brine
  4. dry with materialdried with sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue was chromatographed over alumina

出典と根拠

ORDレコード
ord-55cf9224a7dd44b796f9a12d7042ff05
出典データセット
uspto-grants-1993_04
特許番号
US05206259

反応ノート

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