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

N,N'-Dimethylethylenediamine → (S)-5-(4-fluoro-phenyl)-6-hydroxymethyl-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one

HRID 2046192
노트
인쇄 미리보기

반응식

HRID 2046192 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][CH:3]=1.[O:9]([CH2:16][C:17]1[CH:32]=[C:20]2[C:21](=[O:31])[NH:22][C@H:23]([CH2:25][O:26][Si](C)(C)C)[CH2:24][N:19]2[N:18]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C([O-])([O-])=O.[K+].[K+].CNCCNC>C1(C)C=CC=CC=1.CCOC(C)=O.[Cu]I>[F:8][C:5]1[CH:6]=[CH:7][C:2]([N:22]2[C@H:23]([CH2:25][OH:26])[CH2:24][N:19]3[N:18]=[C:17]([CH2:16][O:9][C:10]4[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=4)[CH:32]=[C:20]3[C:21]2=[O:31])=[CH:3][CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8070N,N'-DimethylethylenediamineHCID 99931-Bromo-4-fluorobenzeneHCID 11430Potassium CarbonateHCID 67976039HCID 67976039, 화합물

생성물 1

HCID 67974066(S)-5-(4-fluoro-phenyl)-6-hydroxymethyl-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one수율 71.8%

시약·촉매·용매 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 1140Toluene용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
140 °C

실험 절차

Copper (I) iodide (41 mg, 0.22 mmol) was added to a stirred suspension of 4-bromofluorobenzene (0.24 mL, 2.17 mmol), (S)-2-phenoxymethyl-6-trimethylsilanyloxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one (0.37 g, 1.08 mmol), K2CO3 (0.3 g, 2.17 mmol) and N,N′-dimethylethylenediamine (0.070 mL, 0.65 mmol) in toluene (8 mL) in a sealed tube and under nitrogen. The mixture was stirred at 140° C. for 24 hours. The mixture was diluted with AcOEt and washed with a 16% aqueous solution of NH4OH. The organic layer was separated, dried (MgSO4), filtered and the solvents evaporated in vacuo. The residue was dissolved in MeOH (4 mL) and stirred at 100° C. for 10 minutes under microwave irradiation. The solvent was evaporated in vacuo and the residue purified by flash column chromatography (silica; AcOEt in DCM 0/100 to 50/50). Desired fractions were collected and the solvents evaporated in vacuo to yield (S)-5-(4-fluoro-phenyl)-6-hydroxymethyl-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one (285 mg, 71% yield) as an off-white foam. 1H NMR (400 MHz, CDCl3) δ ppm 2.21 (br. s., 1H), 3.57-3.68 (m, 1H), 3.81 (dt, J=10.9, 4.4 Hz, 1H), 4.13-4.20 (m, 1H), 4.61 (dd, J=13.4, 4.9 Hz, 1H), 4.81 (dd, J=13.4, 2.1 Hz, 1H), 5.10 (s, 2H), 6.95-7.03 (m, 4H), 7.09-7.18 (m, 2H), 7.27-7.35 (m, 4H).

후처리

  1. washwashed with a 16% aqueous solution of NH4OH
  2. customThe organic layer was separated
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvents evaporated in vacuo
  6. dissolutionThe residue was dissolved in MeOH (4 mL)
  7. stirringstirred at 100° C. for 10 minutes under microwave irradiation
  8. customThe solvent was evaporated in vacuo
  9. customthe residue purified by flash column chromatography (silica; AcOEt in DCM 0/100 to 50/50)
  10. customDesired fractions were collected
  11. customthe solvents evaporated in vacuo

출처 및 근거

ORD 기록
ord-c00831e292cd4cad8610f0788aad389b
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08592422B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트