Sodium Bicarbonate → HCID 178477970, 화합물

HRID 455143

반응식

HRID 455143 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][N:11]3[C:16]=2[CH2:17][C:18]([NH:20][NH2:21])=O)=[CH:4][CH:3]=1.Cl.[N:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[C:29](=N)[NH2:30].C([O-])(O)=O.[Na+]>CN(C=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][N:11]3[C:16]=2[CH2:17][C:18]2[NH:30][C:29]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][N:23]=3)=[N:21][N:20]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 12403615Pyridine-2-carboximidamide hydrochlorideHCID 670291592-(2-(4-Chlorophenyl)imidazo[1,2-a]pyridin-3-yl)acetohydrazide

생성물 1

HCID 178477970HCID 178477970, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

A mixture of 2-(2-(4-chlorophenyl)imidazo[1,2-a]pyridin-3-yl)acetohydrazide (0.55 mmol, 1.0 eq) in DMF (1-2 ml) and picolinimidamide hydrochloride (1.5 eq) was heated at 120° C. for 3 h. The mixture was cooled to rt, treated with sat. NaHCO3 (5 ml), extracted with CH2Cl2 (10 ml). The organic solution was dried with Na2SO4, evaporated under vacuum. The crude product was purified by HPLC. M/e+ 387 for C21H16ClN6 (M+H)+; 1H-NMR (400 MHz, CD3OD) δ 9.11 (d, J=1.4 Hz, 1H), 8.56 (d, J=3.7 Hz, 1H), 8.36 (d, J=6.2 Hz, 2H), 7.77 (d, J=8.4 Hz, 2H), 7.70 (dt, J=8.4, 2.9 Hz, 2H), 7.36 (m, 2H), 6.99 (m, 2H), 4.64 (s, 2H) ppm.

후처리

  1. temperatureThe mixture was cooled to rt
  2. extractionextracted with CH2Cl2 (10 ml)
  3. dry with materialThe organic solution was dried with Na2SO4
  4. customevaporated under vacuum
  5. customThe crude product was purified by HPLC

출처 및 근거

ORD 기록
ord-7298ab0a1a6f476d8420421f50ffba9f
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08497278B2

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