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

Potassium Carbonate → HCID 178488429, 화합물

HRID 641702
노트
인쇄 미리보기

반응식

HRID 641702 반응식
[NH2:1][C:2]1[N:3]=[C:4]([CH3:24])[C:5]2[CH:11]=[C:10](Br)[C:9](=[O:13])[N:8]([C@H:14]3[CH2:19][CH2:18][C@@H:17]([O:20][CH2:21][CH2:22][OH:23])[CH2:16][CH2:15]3)[C:6]=2[N:7]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:31][O:32][C:33]1[CH:38]=[CH:37][C:36](B(O)O)=[CH:35][N:34]=1>[Pd](Cl)Cl>[NH2:1][C:2]1[N:3]=[C:4]([CH3:24])[C:5]2[CH:11]=[C:10]([C:36]3[CH:35]=[N:34][C:33]([O:32][CH3:31])=[CH:38][CH:37]=3)[C:9](=[O:13])[N:8]([C@H:14]3[CH2:19][CH2:18][C@@H:17]([O:20][CH2:21][CH2:22][OH:23])[CH2:16][CH2:15]3)[C:6]=2[N:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2734368(6-Methoxypyridin-3-yl)boronic acidHCID 178433332HCID 178433332, 화합물

생성물 1

HCID 178488429HCID 178488429, 화합물수율 93%

시약·촉매·용매 1

HCID 24290Palladium Chloride촉매

반응 조건

온도
100 °C

실험 절차

A mixture of 2-amino-6-bromo-8-(cis-4-(2-hydroxyethoxy)cyclohexyl)-4-methylpyrido[2,3-d]pyrimidin-7(8H)-one (50 mg, 0.13 mmol), potassium carbonate (52 mg, 0.38 mmol), and 2-methoxy-5-pyridine boronic acid (38 mg, 0.25 mmol) in 5:1 dimethylformade:water (1.3 mL) was bubbled with argon for 5 minutes. To the mixture was added bis(tripehnylphosphine) palladium (II) chloride (9 mg, 0.13 mmol) and the microwave vial was immediately sealed and the mixture was bubbled again with argon. After heating for 20 min at 100° C. in the microwave, the mixture was concentrated in vacuo. The residue was dissolved in CHCl3 (60 mL) and washed with water (10 mL) and brine (10 mL). The organic layer was dried (Na2SO4), filtered and concentrated. The crude product was purified by flash chromatography eluting with chloroform/7 N ammonia in methanol (0-5%) to afford the title compound (50 mg, 93%).

후처리

  1. customwater (1.3 mL) was bubbled with argon for 5 minutes
  2. customthe microwave vial was immediately sealed
  3. customthe mixture was bubbled again with argon
  4. concentrationthe mixture was concentrated in vacuo
  5. dissolutionThe residue was dissolved in CHCl3 (60 mL)
  6. washwashed with water (10 mL) and brine (10 mL)
  7. dry with materialThe organic layer was dried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe crude product was purified by flash chromatography
  11. washeluting with chloroform/7 N ammonia in methanol (0-5%)

출처 및 근거

ORD 기록
ord-1c561698d2d44b5685c50d9348be7067
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07696213B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트