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Carbon Dioxide → N~1~-(4-Methoxyphenyl)ethane-1,2-diamine

HRID 1702496
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인쇄 미리보기

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HRID 1702496 반응식
Cl.[CH3:2][O:3][C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[CH:6][CH:5]=1.O1[CH2:15][CH2:14][NH:13]C1=O.C(=O)=O>COCCOCCO>[CH3:2][O:3][C:4]1[CH:10]=[CH:9][C:7]([NH:8][CH2:15][CH2:14][NH2:13])=[CH:6][CH:5]=1
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참가 물질

5

반응물 3

HCID 280Carbon DioxideHCID 739492-OxazolidinoneHCID 27349564-Anisidine hydrochloride

생성물 1

HCID 12666396N~1~-(4-Methoxyphenyl)ethane-1,2-diamine수율 45%

시약·촉매·용매 1

HCID 8134Diethylene Glycol Monomethyl Ether용매

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온도
175 °C

실험 절차

A mixture of 4-methoxyaniline hydrochloride (17.1 g, 0.107 mole), 2-oxazolidinone (8.7 g, 0.10 mole) and 50 ml of 2-(2-methoxyethoxy)ethanol was heated to 175° C. After five hours, carbon dioxide gas evolution had ceased and the dark mixture was allowed to cool to room temperature. Neutralization in a manner similar to that described in Example 1, and distillation at 130° C. to 140° C. (0.5 mm Hg) afforded a 45 percent yield of the amine as a colorless liquid which slowly solidified on standing at ambient temperature to a low-melting solid.

후처리

  1. temperatureto cool to room temperature
  2. distillationNeutralization in a manner similar to that described in Example 1, and distillation at 130° C. to 140° C. (0.5 mm Hg)

출처 및 근거

ORD 기록
ord-1c37deb58198462a9f94facc94041c26
출처 데이터셋
uspto-grants-1983_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04381401

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