Diethyl (ethoxymethylene)malonate → Diethyl 2-[(4-fluoroanilino)methylene]malonate

반응식

[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[CH:4][CH:3]=1.C(O[CH:12]=[C:13]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])C>>[CH2:17]([O:16][C:14](=[O:15])[C:13](=[CH:12][NH:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1)[C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH3:18]

참가 물질

반응물 2

HCID 6871Diethyl (ethoxymethylene)malonate

HCID 97314-Fluoroaniline

생성물 1

HCID 595792Diethyl 2-[(4-fluoroanilino)methylene]malonate

반응 조건

온도: 100 °C

실험 절차

A mixture of 4-fluoro-phenylamine (5.1 mL, 54.4 mmol) and diethyl ethoxymethylenemalonate (10 mL, 49.5 mmol) was heated at 100° C. for 4 hours, an oil which solidified on cooling. The solid was triturated in heptane, collected by filtration and washed with heptane, to give the product as a colorless solid, 10.5 g (75%). MS: m/z 282.1 (MH+).

후처리

temperatureon cooling
customThe solid was triturated in heptane
filtrationcollected by filtration
washwashed with heptane

출처 및 근거

ORD 기록: ord-3b66e682b83f455f8328c78b7d89b47d
출처 데이터셋: uspto-grants-2013_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08394828B2

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