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

HRID 1869929노트

반응식

HRID 1869929 반응식
[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

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 21107262N-[(3-iodophenyl)methyl]cyclopropanamine2회

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-b3b95d6918b84e9cab2f31d7458c9d89
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07638648B2

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