2-Methoxyethylamine → beta-[(2-Methoxyethyl)amino]-alpha-phenylbenzeneethanol

HRID 1381521

반응식

HRID 1381521 반응식
[C:1]1([CH:7]2[O:15][CH:8]2[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:16][O:17][CH2:18][CH2:19][NH2:20]>O>[CH3:16][O:17][CH2:18][CH2:19][NH:20][CH:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[CH:8]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[OH:15]

참가 물질

4

반응물 2

HCID 80182-MethoxyethylamineHCID 28649Stilbene oxide2회

생성물 1

HCID 411476beta-[(2-Methoxyethyl)amino]-alpha-phenylbenzeneethanol수율 80%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

A mixture of trans-stilbene oxide (3.93 g, 0.020 mole) and 2-methoxyethylamine (4.51 g, 0.060 mole) was heated at 125° C. for 2 hours with an oil bath. A mass spectra analysis showed no title compound was present. The mixture was heated for another 2 hours at 150° C. The mixture was poured into water (using methanol rinse) to obtain an off-white solid. NMR analysis showed the solid contained approximately 60% unreacted stilbene oxide. The mixture was added to another 4.51 g (0.060 mole) of 2-methoxy ethylamine and the mixture heated at 135° C. for 4 hours in a stainless-steel bomb. After cooling, the reaction mixture was shown by NMR analysis to contain 20% stilbene oxide and 80% of the title compound. The solid was recrystallized from toluene to give 2.92 g (54%) of a white solid, m.p. 137°-139° C.

후처리

  1. customto obtain an off-white solid
  2. temperatureAfter cooling

출처 및 근거

ORD 기록
ord-ddd1ff081f7947d5957272c46c029e9e
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04803200

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