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

Potassium Phosphate, Tribasic → 3-[3-(7-Formylimidazo[1,2-alpha]pyridin 3-yl)phenyl]thiophene-2-carbonitrile

HRID 985536
노트
인쇄 미리보기

반응식

HRID 985536 반응식
Br[C:2]1[N:6]2[CH:7]=[CH:8][C:9]([CH:11]=[O:12])=[CH:10][C:5]2=[N:4][CH:3]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].CC1(C)C(C)(C)OB([C:29]2[CH:30]=[C:31]([C:35]3[CH:39]=[CH:38][S:37][C:36]=3[C:40]#[N:41])[CH:32]=[CH:33][CH:34]=2)O1>CN(C)C(=O)C.O.C(=O)([O-])O.[Na+]>[CH:11]([C:9]1[CH:8]=[CH:7][N:6]2[C:2]([C:33]3[CH:32]=[C:31]([C:35]4[CH:39]=[CH:38][S:37][C:36]=4[C:40]#[N:41])[CH:30]=[CH:29][CH:34]=3)=[CH:3][N:4]=[C:5]2[CH:10]=1)=[O:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 225070883-[3-(4,4,5,5-Tetramethyl-[1,3,2]dioxaborolan-2-yl)phenyl]thiophene-2-carbonitrileHCID 768496803-Bromoimidazo[1,2-A]pyridine-7-carbaldehyde

생성물 1

HCID 99020133-[3-(7-Formylimidazo[1,2-alpha]pyridin 3-yl)phenyl]thiophene-2-carbonitrile수율 68%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 31374Dimethylacetamide용매
HCID 516892Sodium Bicarbonate용매

반응 조건

온도
80 °C

실험 절차

3-Bromoimidazo[1,2-α]pyridine-7-carboxaldehyde (1.15 g, 5.16 mmol), potassium phosphate (2.19 g, 10.31 mmol) and 3-[3-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)phenyl]thiophene-2-carbonitrile (2.58 g, 8.26 mmol) were dissolved in N,N-dimethylacetamide (15 ml) and the mixture degassed with N2 for 15 min. Tetrakis(triphenylphosphine)pallidum(0) (0.30 g, 0.26 mmol) was added and the mixture heated at 80° C. for 18 h. The mixture was allowed to cool to room temperature, diluted with water (20 ml) and saturated sodium hydrogencarbonate solution (20 ml), then extracted with ethyl acetate (2×75 ml). The combined organic fractions were washed with brine (40 ml), dried over anhydrous sodium sulfate and evaporated to give a black oil. The oil was purified by silica gel chromatography eluting with dichloromethane and 1% conc. ammonia on a gradient of methanol (1-2%). The solid obtained was triturated with diethyl ether which gave the title compound (1.15 g, 68%) as a white powder. Oxalate salt, white powder. 1H NMR (360 MHz, d6-DMSO) δH 7.30 (1H, dd, J 7 and 1), 7.70-7.88 (4H, m), 8.08 (1H, s), 8.16-8.22 (2H, m), 8.44 (1H, s), 8.78 (1H, d, J 7), 10.05 (1H, s); m /z (ES+) 330 (M++H).

후처리

  1. customthe mixture degassed with N2 for 15 min
  2. temperatureto cool to room temperature
  3. extractionextracted with ethyl acetate (2×75 ml)
  4. washThe combined organic fractions were washed with brine (40 ml)
  5. dry with materialdried over anhydrous sodium sulfate
  6. customevaporated
  7. customto give a black oil
  8. customThe oil was purified by silica gel chromatography
  9. washeluting with dichloromethane and 1% conc. ammonia on a gradient of methanol (1-2%)
  10. customThe solid obtained
  11. customwas triturated with diethyl ether which

출처 및 근거

ORD 기록
ord-a8a221c07de14e5789a0b6fe31606d20
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06872731B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트