홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

1,2-Dichloroethane → N-(4-(2,3-difluorophenylamino)pyridin-3-yl)-2-fluoropyridine-3-carboxamide

HRID 253971
노트
인쇄 미리보기

반응식

HRID 253971 반응식
[F:1][C:2]1[C:7]([C:8]([OH:10])=O)=[CH:6][CH:5]=[CH:4][N:3]=1.C1C=CC2N(O)N=NC=2C=1.CCN(CC)CC.[F:28][C:29]1[C:34]([F:35])=[CH:33][CH:32]=[CH:31][C:30]=1[NH:36][C:37]1[CH:42]=[CH:41][N:40]=[CH:39][C:38]=1[NH2:43].C(Cl)CCl>CN(C=O)C.O>[F:28][C:29]1[C:34]([F:35])=[CH:33][CH:32]=[CH:31][C:30]=1[NH:36][C:37]1[CH:42]=[CH:41][N:40]=[CH:39][C:38]=1[NH:43][C:8]([C:7]1[C:2]([F:1])=[N:3][CH:4]=[CH:5][CH:6]=1)=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 960892-Fluoronicotinic acidHCID 58179850N4-(2,3-difluorophenyl)pyridine-3,4-diamine

생성물 1

HCID 58179455N-(4-(2,3-difluorophenylamino)pyridin-3-yl)-2-fluoropyridine-3-carboxamide수율 45%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회

반응 조건

온도
0 °C

실험 절차

To a solution of 2-fluoropyridine-3-carboxylic acid (1.41 g, 10.00 mmol) in anhydrous DMF (15 mL) was added HOBT (2.56 g, 16.74 mmol) and Et3N (2.0 g, 20.09 mmol) at RT. The mixture was cooled to 0° C., treated with a solution of N4-(2,3-difluorophenyl)pyridine-3,4-diamine in DMF (15 mL), stirred for 15 min at RT and EDC (3.2 g, 16.74 mmol) was added portion wise. The reaction mixture was warmed to RT and stirred for 16 hr. The reaction mixture was diluted with water (100 mL) and extracted with EtOAc (4×200 mL). The combined organics were washed with saturated aq. NaHCO3 solution (2×100 mL), water (2×100 mL), brine solution (100 mL), and dried (Na2SO4). Filtration and evaporation of the solvent in vacuo gave a brown solid. Chromatographic purification (silica gel, 1% methanol in chloroform) provided N-(4-(2,3-difluorophenylamino)pyridin-3-yl)-2-fluoropyridine-3-carboxamide (1.05 g, 45% yield) as yellow solid; LC-MS: 345.2 (M+H).

후처리

  1. temperatureThe reaction mixture was warmed to RT
  2. stirringstirred for 16 hr
  3. extractionextracted with EtOAc (4×200 mL)
  4. washThe combined organics were washed with saturated aq. NaHCO3 solution (2×100 mL), water (2×100 mL), brine solution (100 mL)
  5. dry with materialdried (Na2SO4)
  6. filtrationFiltration and evaporation of the solvent in vacuo
  7. customgave a brown solid
  8. customChromatographic purification (silica gel, 1% methanol in chloroform)

출처 및 근거

ORD 기록
ord-a5a4444d8fa44a67bc00ec62301270f6
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07872031B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트