Potassium Carbonate → HCID 178479536, 화합물

HRID 606925노트

반응식

HRID 606925 반응식
[ClH:1].[NH2:2][OH:3].[C:4]1([C:10]#[C:11][C:12]2[CH:13]=[N:14][CH:15]=[C:16]([CH:19]=2)[C:17]#[N:18])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C(=O)([O-])[O-].[K+].[K+]>>[ClH:1].[OH:3][NH:2][C:17](=[NH:18])[C:16]1[CH:19]=[C:12]([C:11]#[C:10][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:13]=[N:14][CH:15]=1

참가 물질

4

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 28223905-(2-phenylethynyl)nicotinonitrile

생성물 1

HCID 178479536HCID 178479536, 화합물

실험 절차

Add hydroxylamine hydrochloride (0.55 g, 7.8 mmol) to a suspension of 5-phenylethynylnicotinonitrile (0.20 g, 0.98 mmol) and potassium carbonate (0.68 g, 4.9 mmol) and heat at reflux for 2 h. Cool the reaction mixture to room temperature, filter away any solids and concentrate. Purify by silica gel chromatography, eluting with 40:60 ethyl acetate:hexanes, to obtain the free base of the title compound as a white solid. Dissolve the free base in diethyl ether, add a 1 M solution of hydrogen chloride in diethyl ether (1.1 eq) and collect the resulting precipitated solids by filtration to give the title compound (0.1 g, 37%).

후처리

  1. temperatureheat
  2. temperatureat reflux for 2 h
  3. filtrationfilter away any solids
  4. concentrationconcentrate
  5. customPurify by silica gel chromatography
  6. washeluting with 40:60 ethyl acetate

출처 및 근거

ORD 기록
ord-8e8b99c73b8f4acab72ed0a28467d69a
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915424B2

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