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

Sodium Carbonate → HCID 57537662, 화합물

HRID 1693721
노트
인쇄 미리보기

반응식

HRID 1693721 반응식
Br[C:2]1[CH:3]=[C:4]([CH:8]([OH:14])[C:9]([N:11]([CH3:13])[CH3:12])=[O:10])[CH:5]=[N:6][CH:7]=1.C([O-])(=O)C.[K+].Br[C:21]1[C:22]([C:46]([F:49])([F:48])[F:47])=[C:23]2[C:29]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=3[O:36][CH3:37])=[CH:28][N:27](COCC[Si](C)(C)C)[C:24]2=[N:25][CH:26]=1.C(=O)([O-])[O-].[Na+].[Na+].S([O-])([O-])(=O)=O.[Na+].[Na+]>CC(N(C)C)=O>[OH:14][CH:8]([C:4]1[CH:5]=[N:6][CH:7]=[C:2]([C:21]2[C:22]([C:46]([F:47])([F:48])[F:49])=[C:23]3[C:29]([C:30]4[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=4[O:36][CH3:37])=[CH:28][NH:27][C:24]3=[N:25][CH:26]=2)[CH:3]=1)[C:9]([N:11]([CH3:13])[CH3:12])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 10340Sodium CarbonateHCID 24436Sodium SulfateHCID 517044Potassium AcetateHCID 57537548HCID 57537548, 화합물HCID 57537619HCID 57537619, 화합물

생성물 1

HCID 57537662HCID 57537662, 화합물수율 7%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A mixture of 2-(5-Bromo-pyridin-3-yl)-2-hydroxy-N,N-dimethyl-acetamide (40 mg, 0.15 mmol), bis(pinacol)diborane (47 mg, 0.18 mmol), potassium acetate (45 mg, 0.46 mmol), and 1,1′-bis(diphenylphosphino)ferrocenepalladium(II)-dichloride dichlormethane adduct (6 mg, 0.007 mmol) in dimethylacetamide (1 mL) was irradiated in a Personal Chemistry Optimizer at 120° C. for 30 min. 5-Bromo-3-(2-methoxy-phenyl)-4-trifluoromethyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrrolo[2,3-b]pyridine (39 mg, 0.077 mmol), sodium carbonate solution (2M in water, 0.39 mL, 0.77 mmol), and additional 1,1′-bis(diphenylphosphino)ferrocenepalladium(II)-dichloride dichlormethane adduct (3 mg, 0.03 mmol) was added and the mixture was irradiated for an additional 30 min at 120° C. Sodium sulfate was added to the crude reaction mixture and the solids were filtered over Celite. The solids were rinsed with ethyl acetate and the combined filtrate was concentrated. The solids were resuspended in ethyl acetate, filtered through a plug of silica and the eluent was concentrated. The resulting oil was dissolved in trifluoroacetic acid (2 mL) and shaken for 5 min. The solution was concentrated and the mixture was redissolved in dimethyl sulfoxide and ethylenediamine. Purification by mass triggered reverse phase HPLC afforded 2-Hydroxy-2-{5-[3-(2-methoxy-phenyl)-4-trifluoromethyl-1H-pyrrolo[2,3-b]pyridin-5-yl]-pyridin-3-yl}-N,N-dimethyl-acetamide (2.5 mg, 0.005 mmol, 7% yield). 1H NMR (500 MHz, MeOH-d4) δ 12.55 (bs, 1H), 8.60 (s, 1H), 8.51 (s, 1H), 8.24 (s, 1H), 7.72 (s, 1H), 7.71 (m, 1H), 7.31 (m, 1H), 7.24 (dd, J=7 Hz, J2=2 Hz, 1H), 6.99 (d, J=7.5 Hz, 1H), 6.95 (td, J=7.5 Hz, J2=1 Hz, 1H), 5.8 (bs, 1H), 5.56 (s, 1H), 3.65 (s, 3H), 2.90 (m, 3H), 2.84 (s, 3H). MS: m/z 471.0 (M+H+).

후처리

  1. customwas irradiated in a Personal Chemistry Optimizer at 120° C. for 30 min
  2. customthe mixture was irradiated for an additional 30 min at 120° C
  3. customreaction mixture
  4. filtrationthe solids were filtered over Celite
  5. washThe solids were rinsed with ethyl acetate
  6. concentrationthe combined filtrate was concentrated
  7. filtrationfiltered through a plug of silica
  8. concentrationthe eluent was concentrated
  9. dissolutionThe resulting oil was dissolved in trifluoroacetic acid (2 mL)
  10. concentrationThe solution was concentrated
  11. dissolutionthe mixture was redissolved in dimethyl sulfoxide
  12. customPurification by mass triggered reverse phase HPLC

출처 및 근거

ORD 기록
ord-e887dd6a627c40ba8143286cb8aaab47
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08158647B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트