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

Propargyl alcohol → HCID 12083033, 화합물

HRID 1168508
노트
인쇄 미리보기

반응식

HRID 1168508 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C([Li])CCC.Br[C:26]1[CH:27]=[C:28]2[C:33]3=[C:34]([CH2:36][C:37]([CH3:39])([CH3:38])[N:32]3[CH:31]=[C:30]([C:40]([O:42][CH2:43][CH3:44])=[O:41])[C:29]2=[O:45])[CH:35]=1.[CH2:46]([OH:49])[C:47]#[CH:48]>C1COCC1.C(NCC)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.[Cu](I)I>[OH:49][CH2:46][C:47]#[C:48][C:26]1[CH:27]=[C:28]2[C:33]3=[C:34]([CH2:36][C:37]([CH3:39])([CH3:38])[N:32]3[CH:31]=[C:30]([C:40]([O:42][CH2:43][CH3:44])=[O:41])[C:29]2=[O:45])[CH:35]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 7859Propargyl alcoholHCID 11776TriphenylphosphineHCID 12083032ethyl 8-bromo-2,2-dimethyl-6-oxo-1,2-dihydro-6H-pyrrolo[3,2,1-ij]quinoline-5-carboxylateHCID 178418339Butyllithium

생성물 1

HCID 12083033HCID 12083033, 화합물

시약·촉매·용매 4

HCID 83717Copper iodide
촉매
HCID 167845palladium(II) acetate촉매
HCID 8021Diethylamine용매
HCID 8028Tetrahydrofuran용매

반응 조건

온도
22 °C

실험 절차

A solution of palladium acetate (73 mg) and triphenyl phosphine (191 mg) in dry THF (6.0 mL) under nitrogen is cooled to 0° C. A solution of n-butyllithium (1.6 M in hexanes, 444 μL) is added dropwise and after 15 min, the solution is warmed to 22° C. for 15 min. The solution is then canulated into a mixture of ethyl 8-bromo-2,2-dimethyl-6-oxo-1,2-dihydro-6H-pyrrolo[3,2,1-ij]quinoline-5-carboxylate (Preparation 13, 350 mg), copper iodide (84 mg) and propargyl alcohol (75 μL) in diethylamine (6.0 mL). The reaction is warmed to 45° C. for 2 hours. The reaction is filtered, diluted with CH2Cl2 (100 mL), and washed with water. The organic layer is dried (MgSO4), filtered, and concentrated. The crude product is chromatographed over silica gel, eluting with 5% MeOH in CHCl3 and recrystallized from EtOAc to afford 229 mg of the title compound as white crystals. Physical characteristics: M.p. 237° C. (dec); 1H NMR (DMSO-d6) δ8.74, 7.81, 7.60, 5.37, 4.33, 4.23, 3.39, 1.63 (s, 6 H), 1.29 (t, J=7 Hz, 3 H); IR (diffuse reflectance) 2391, 2222, 2058, 1921, 1680, 1637, 1595, 1542, 1510, 1317, 1216, 1186, 1040, 1031, 808 cm−1; MS (EI) m/z 325 (M+). HRMS (FAB) m/z 326.1385 (C19H19NO4+H).

후처리

  1. temperatureThe reaction is warmed to 45° C. for 2 hours
  2. filtrationThe reaction is filtered
  3. additiondiluted with CH2Cl2 (100 mL)
  4. washwashed with water
  5. dry with materialThe organic layer is dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude product is chromatographed over silica gel
  9. washeluting with 5% MeOH in CHCl3
  10. customrecrystallized from EtOAc

출처 및 근거

ORD 기록
ord-0e66815af6544d0cb65813a957abd6a8
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06624159B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트