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Methylamine → [2-(2-Methoxyphenoxy)ethyl](methyl)amine

HRID 2297569
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HRID 2297569 반응식
Br[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[O:11][CH3:12].[CH3:13][NH2:14]>C(O)C>[CH3:12][O:11][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[O:4][CH2:3][CH2:2][NH:14][CH3:13]
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 17990992-(2-Bromoethoxy)anisole

생성물 1

HCID 6485441[2-(2-Methoxyphenoxy)ethyl](methyl)amine수율 98%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 1-(2-bromoethoxy)-2-methoxybenzene (7d) (7.7 g, 33 mmol) in a 33% solution of methylamine in ethanol was heated at 80° C. in a sealed tube for 16 h. After cooling to room temperature, the solvents were evaporated in vacuo. A 2N aqueous solution of sodium hydroxide was added to the remaining oil and the resulting slurry was extracted with ethyl acetate (2×250 mL). The collected organic phases were dried (Na2SO4) and the solvents evaporated in vacuo giving 5.9 g (98%) of the title compound as an oil: 1H NMR (CDCl3) δ 1.85 (broad s, 1H), 2.50 (s, 3H), 3.00 (t, 2H), 3.85 (s, 3H), 4.10 (t, 2H), 6.85-6.95 (m, 4H).

후처리

  1. customthe solvents were evaporated in vacuo
  2. additionA 2N aqueous solution of sodium hydroxide was added to the remaining oil
  3. extractionthe resulting slurry was extracted with ethyl acetate (2×250 mL)
  4. dry with materialThe collected organic phases were dried (Na2SO4)
  5. customthe solvents evaporated in vacuo

출처 및 근거

ORD 기록
ord-4c46427fac9a43dbbac67362b16ecd82
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06492374B2

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