Diethyl Ether → Cyclopropyl-(3-iodo-benzyl)-methyl-amine

HRID 1869929ノート

反応式

HRID 1869929 の反応式
[CH:1]1([NH:4][CH2:5][C:6]2[CH:11]=[CH:10][CH:9]=[C:8]([I:12])[CH:7]=2)[CH2:3][CH2:2]1.[C:13](=O)([O-])[O-].[K+].[K+].CI.C(OCC)C>CC(C)=O>[CH:1]1([N:4]([CH2:5][C:6]2[CH:11]=[CH:10][CH:9]=[C:8]([I:12])[CH:7]=2)[CH3:13])[CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 21107262N-[(3-iodophenyl)methyl]cyclopropanamine2 回

生成物 1

HCID 21107263Cyclopropyl-(3-iodo-benzyl)-methyl-amine収率 77%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A solution of cyclopropyl-(3-iodo-benzyl)-amine (Intermediate 88, 4.1 g, 151 mmol) in acetone (20 mL) was treated with potassium carbonate (2.07 g, 15 mmol) and methyl iodide (1.4 mL, 22.5 mmol) and the resulting reaction mixture was stirred at ambient temperature for 1 h. Diethyl ether was added, the solids were filtered off and filtrate was evaporated to a residue that was subjected to flash column chromatography over silica gel (230-400 mesh) using 10% ethyl acetate in hexane as the eluent to afford the title compound (3.3 g, 77%).

後処理

  1. customthe resulting reaction mixture
  2. filtrationthe solids were filtered off
  3. customfiltrate was evaporated to a residue that

出典と根拠

ORDレコード
ord-b3b95d6918b84e9cab2f31d7458c9d89
出典データセット
uspto-grants-2009_12
特許番号
US07638648B2

反応ノート

読み込み中…