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

Oxalic Acid → HCID 59454955, 화합물

HRID 1400491
노트
인쇄 미리보기

반응식

HRID 1400491 반응식
[CH3:1][CH:2]1[C:14]2[C:13]3[CH:12]=[C:11]([CH3:15])[CH:10]=[CH:9][C:8]=3[NH:7][C:6]=2[CH2:5][CH:4]([CH3:16])[N:3]1[CH3:17].P([O-])([O-])([O-])=O.[K+].[K+].[K+].Br[CH:27]=[C:28]([C:33]1[CH:38]=[CH:37][N:36]=[CH:35][CH:34]=1)[C:29](C)(C)C.C(O)(=O)C(O)=O>CN(C=O)C.C1COCC1.N1CCC[C@H]1C(O)=O.[Cu]I>[CH3:1][CH:2]1[C:14]2[C:13]3[CH:12]=[C:11]([CH3:15])[CH:10]=[CH:9][C:8]=3[N:7](/[CH:27]=[C:28](/[C:33]3[CH:38]=[CH:37][N:36]=[CH:35][CH:34]=3)\[CH3:29])[C:6]=2[CH2:5][CH:4]([CH3:16])[N:3]1[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 971Oxalic AcidHCID 62657Potassium Phosphate, TribasicHCID 67309717HCID 67309717, 화합물HCID 86644760HCID 86644760, 화합물

생성물 1

HCID 59454955HCID 59454955, 화합물

시약·촉매·용매 3

HCID 67304547HCID 67304547, 화합물촉매
HCID 6228
Dimethylformamide
용매
HCID 8028Tetrahydrofuran용매

실험 절차

2,3,4,5-Tetrahydro-1,2,3,8-tetramethyl-1H-pyrido[4,3-b]indole (550 mg, 2 mmol) was dissolved in DMF. Copper (I) iodide L-proline (46 mg, 0.4 mmol) and potassium phosphate (848 mg, 4 mmol) were added and the reaction mixture was stirred for 10 min. at RT. 4-(1-bromo-3,3-dimethylbut-1-en-2-yl)pyridine (294 mg, 3.0 mmol) was added dropwise and the reaction mixture was purged with nitrogen. The reaction mixture was heated overnight at 85° C. (prolonged heating in some cases was required). DMF was evaporated under reduced pressure, the residue was diluted with water and the solid was filtered. The solid material was purified by silica gel chromatography (100-200 mesh). The product was further purified by HPLC. The free base was converted into oxalate salt by treatment of oxalic acid (1 equiv) in THF. Yield: 8 mg as the oxalate salt. 1H NMR (CD3OD, freebase) δ (ppm): 8.60 (d, 2H), 7.70 (d, 2H), 7.35 (s, 1H), 7.30 (s, 1H), 7.10 (m, 2H), 4.50 (m, 1H), 4.0 (m, 1H), 3.10 (m, 1H), 2.90 (s, 3H), 2.80 (m, 1H), 2.42 (s, 3H), 2.0 (s, 3H), 1.76 (d, 3H), 1.50 (d, 3H).

후처리

  1. customthe reaction mixture was purged with nitrogen
  2. temperatureThe reaction mixture was heated overnight at 85° C. (
  3. temperatureprolonged heating in some cases
  4. customDMF was evaporated under reduced pressure
  5. additionthe residue was diluted with water
  6. filtrationthe solid was filtered
  7. customThe solid material was purified by silica gel chromatography (100-200 mesh)
  8. customThe product was further purified by HPLC

출처 및 근거

ORD 기록
ord-f4b5ff8540b640499c2bf99b0162b270
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08906925B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트