Ammonium Hydroxide → HCID 19851786, 화합물

HRID 1607042노트

반응식

HRID 1607042 반응식
[N:1]1[C:10]2[CH:9]([CH2:11][CH2:12][CH2:13][N:14]3[C:18]4=[N:19][CH:20]=[C:21]([CH2:23][C:24]5[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=5)[CH:22]=[C:17]4N=N3)[CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[OH-:30].[NH4+]>O>[N:1]1[C:10]2[CH:9]([CH2:11][CH2:12][CH2:13][NH:14][C:18]3[C:17]([OH:30])=[CH:22][C:21]([CH2:23][C:24]4[CH:25]=[N:26][CH:27]=[CH:28][CH:29]=4)=[CH:20][N:19]=3)[CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 14923Ammonium HydroxideHCID 198517953-(5,6,7,8-Tetrahydroquinol-8-yl)propyl-6-(pyrid-3-ylmethyl)-3H-1,2,3-triazolo[5,4-b]pyridine

생성물 1

HCID 19851786HCID 19851786, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3-[3-(5,6,7,8-tetrahydroquinol-8-yl)-propyl]-6-(pyrid-3-ylmethyl)-3H-1,2,3-triazolo[5,4-b]-pyridine (3.56 g) and polyphosphoric acid (17.5 g) were heated with stirring at 188°-197° C. for 50 minutes. Water (30 ml) was added to the hot residue and, after slight cooling, the solution was basified with aqueous ammonium hydroxide to pH 10 and then extracted with chloroform. The combined chloroform extracts were dried over magnesium sulphate, concentrated in vacuo and the residue was chromatographed on silica eluted with 5% v/v methanol in chloroform to give the title compound as a brown gum (0.68 g). The aqueous portion after extraction, was concentrated to dryness, to give a paste, water (100 ml) was then added, the mixture was refluxed for 1 hour and a brown oil which formed was extracted with chloroform (3 x 100 ml). The extracts were dried, combined and concentrated to give a further quantity of the title compound as an oil (0.31 g). The two portions of the product were combined, converted to the trihydrochloride with ethanolic HCl and then recrystallised, first from isopropanol and then from isopropanol/methanol to give the title compound as a buff solid (0.5 g).

후처리

  1. temperaturewere heated
  2. extractionextracted with chloroform
  3. dry with materialThe combined chloroform extracts were dried over magnesium sulphate
  4. concentrationconcentrated in vacuo
  5. customthe residue was chromatographed on silica
  6. washeluted with 5% v/v methanol in chloroform

출처 및 근거

ORD 기록
ord-01d6854f6d1942159e0285aa71aed795
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04863933

반응 노트

불러오는 중…