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Dimethylamine, hydrochloride → 7-Methoxy-4-(dimethylaminomethyl)coumarin

HRID 1167051
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반응식

HRID 1167051 반응식
Cl.[CH3:2][NH:3][CH3:4].Br[CH2:6][C:7]1[C:16]2[C:11](=[CH:12][C:13]([O:17][CH3:18])=[CH:14][CH:15]=2)[O:10][C:9](=[O:19])[CH:8]=1.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH3:18][O:17][C:13]1[CH:12]=[C:11]2[C:16]([C:7]([CH2:6][N:3]([CH3:4])[CH3:2])=[CH:8][C:9](=[O:19])[O:10]2)=[CH:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10473Dimethylamine, hydrochlorideHCID 11430Potassium CarbonateHCID 1218944-Bromomethyl-7-methoxycoumarin

생성물 1

HCID 89318307-Methoxy-4-(dimethylaminomethyl)coumarin수율 55.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of dimethylamine hydrochloride (0.18 g), 4-bromomethyl-7-methoxycoumarin (0.30 g), potassium carbonate (0.5 g) and dichloromethane (10 ml) was stirred at room temperature for 2 days. The solid was filtered off and the filtrate concentrated. The residue was purified by chromatography on silica gel (eluent 5% methanol in dichloromethane), then crystallised from methanol to give the title compound as a white solid (0.145 g).

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후처리

  1. filtrationThe solid was filtered off
  2. concentrationthe filtrate concentrated
  3. customThe residue was purified by chromatography on silica gel (eluent 5% methanol in dichloromethane)
  4. customcrystallised from methanol

출처 및 근거

ORD 기록
ord-375bfc90cbe34f90a54dbf2085e3f707
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06617124B1

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