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

Diisopropylethylamine → 6-(methyloxy)-1-(1-methyl-L-prolyl)-7-nitro-1,2,3,4-tetrahydroquinoline

HRID 1014384
노트
인쇄 미리보기

반응식

HRID 1014384 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[N+:13]([O-:15])=[O:14])[NH:9][CH2:8][CH2:7][CH2:6]2.[CH3:16][N:17]1[CH2:24][CH2:23][CH2:22][C@H:18]1[C:19](O)=[O:20].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C)C=O.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[N+:13]([O-:15])=[O:14])[N:9]([C:19](=[O:20])[C@@H:18]1[CH2:22][CH2:23][CH2:24][N:17]1[CH3:16])[CH2:8][CH2:7][CH2:6]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 643474N-Methyl-L-prolineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 594419086-(Methyloxy)-7-nitro-1,2,3,4-tetrahydroquinoline

생성물 1

HCID 673160066-(methyloxy)-1-(1-methyl-L-prolyl)-7-nitro-1,2,3,4-tetrahydroquinoline
수율 45.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 6-(methyloxy)-7-nitro-1,2,3,4-tetrahydroquinoline (3.0 g, 14.41 mmol), 1-methyl-L-proline (2.140 g, 16.57 mmol), HATU (7.12 g, 18.73 mmol), and DIPEA (6.29 mL, 36.0 mmol) in N,N-Dimethylformamide (DMF) (25 mL) was stirred for 2.5 days at room temperature. Reaction was poured into ethyl acetate and washed successively with 5% lithium chloride (aq) and saturated sodium chloride (aq). The organic layer was dried over sodium sulfate, filtered, and purified by column chromatography (10% MeOH/CH2Cl2) to afford 6-(methyloxy)-1-(1-methyl-L-prolyl)-7-nitro-1,2,3,4-tetrahydroquinoline (2.09 g, 6.54 mmol, 45.4% yield). The residue was suspended in ethanol (300 mL) and N,N-dimethylacetamide (50 mL) was added followed by tin(II)chloride dihydrate (6.78 g, 30.1 mmol) and 1.0M HCl (2.505 mL, 2.505 mmol). After overnight stirring the reaction was quenched with excess saturated NaHCO3 (300 mL) and allowed to stir at rt for 30 min. The solids were removed through a celite pad, rinsed with Me0H, and evaporated. The aqueous layer was extracted with DCM (2×100 mL). The combined organic layers were filtered through a cotton plug, and concentrated by rotary evaporation to provide 6-(methyloxy)-1-(1-methyl-L-prolyl)-1,2,3,4-tetrahydro-7-quinolinamine (1.1 g, 26% over two steps). ESIMS (M+H)+=290.

후처리

  1. customReaction
  2. washwashed successively with 5% lithium chloride (aq) and saturated sodium chloride (aq)
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. custompurified by column chromatography (10% MeOH/CH2Cl2)

출처 및 근거

ORD 기록
ord-ba1cfec827df4b949d1cecfbb7cf749b
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981903B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트