Ammonia → 4-Vinylbenzylamine (stabilized with MEHQ)

반응식

[CH:1]([CH:3](Cl)[C:4]1[CH:9]=CC=[CH:6][CH:5]=1)=C.[NH3:11].[Cl-].[NH4+].[CH:14](O)([CH3:16])[CH3:15]>>[NH2:11][CH2:15][C:14]1[CH:16]=[CH:9][C:4]([CH:3]=[CH2:1])=[CH:5][CH:6]=1

참가 물질

반응물 4

HCID 222Ammonia

HCID 3776Isopropanol

HCID 25517Ammonium Chloride

HCID 11768772Benzene, 1-(chloromethyl)-3(or 4)-ethenyl-

생성물 1

HCID 110734664-Vinylbenzylamine (stabilized with MEHQ)

실험 절차

To a 250 mL flask was added vinylbenzyl chloride (7.63 g, 0,050 mol), concentrated aqueous ammonia (9.8 mL), and isopropanol (40 mL). The mixture was stirred for one week, at which point a large quantity of crystalline material (ammonium chloride) had precipitated. The solid was filtered off and washed with isopropanol. The mother liquor was evaporated on a rotary evaporator until no ammonia odor could be detected. Isopropanol (50 mL) was then added, and the mixture refrigerated for several hours. Following refrigeration, ammonium chloride which had precipitated was filtered off to yield 4-aminomethylstyrene which was used without further purification.

후처리

customhad precipitated
filtrationThe solid was filtered off
washwashed with isopropanol
customThe mother liquor was evaporated on a rotary evaporator until no ammonia odor
additionIsopropanol (50 mL) was then added
waitthe mixture refrigerated for several hours
customhad precipitated
filtrationwas filtered off

출처 및 근거

ORD 기록: ord-d5bfa1785a684db4a4aa0fd977bde61d
출처 데이터셋: uspto-grants-1997_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05624963

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