Hydrochloric Acid → HCID 178488956, 화합물

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[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][C:3]=1[O:9][CH3:10].[C:11](O)(=O)[CH:12]([CH3:14])[OH:13].Cl.[OH-].[NH4+]>>[OH:13][CH:12]([C:14]1[NH:1][C:2]2[C:3]([O:9][CH3:10])=[CH:4][CH:5]=[CH:6][C:7]=2[N:8]=1)[CH3:11]

참가 물질

반응물 4

HCID 313Hydrochloric Acid

HCID 612Lactic Acid

HCID 14923Ammonium Hydroxide

HCID 1842683-Methoxybenzene-1,2-diamine

생성물 1

HCID 178488956HCID 178488956, 화합물

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온도: 100 °C

실험 절차

2,3-Diaminoanisole (5.88 g) and lactic acid (5.6 ml) were combined, treated with concentrated hydrochloric acid (45 ml) and heated at 100° C. for 18 h. The reaction was cooled to 0° C., neutralised with ammonium hydroxide solution and extracted with ethyl acetate (3×45 ml). The combined organic layers were dried over magnesium sulphate, filtered and the filtrate evaporated in vacuo and the residue purified by flash chromatography on silica eluting with ethyl acetate to yield the desired product as a reddish-brown solid (4.91 g).

후처리

temperatureThe reaction was cooled to 0° C.
extractionextracted with ethyl acetate (3×45 ml)
dry with materialThe combined organic layers were dried over magnesium sulphate
filtrationfiltered
customthe filtrate evaporated in vacuo
customthe residue purified by flash chromatography on silica eluting with ethyl acetate

출처 및 근거

ORD 기록: ord-5b28579291ae4976832c8cc0540a95c1
출처 데이터셋: uspto-grants-2002_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06353010B1

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