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P,P-Diphenylphosphinic azide → 6-[5-(1-Amino-cyclopropyl)-pyridin-3-yl]-1-methyl-1H-quinolin-2-one

HRID 1774888
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HRID 1774888 반응식
[CH3:1][N:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]3[CH:13]=[C:14]([C:18]4(C(O)=O)[CH2:20][CH2:19]4)[CH:15]=[N:16][CH:17]=3)=[CH:9][CH:10]=2)[CH2:5][CH2:4][C:3]1=[O:24].C1(P([N:39]=[N+]=[N-])(C2C=CC=CC=2)=O)C=CC=CC=1.CC([O-])(C)C.[K+]>C1(C)C=CC=CC=1.C1COCC1>[NH2:39][C:18]1([C:14]2[CH:13]=[C:12]([C:8]3[CH:7]=[C:6]4[C:11](=[CH:10][CH:9]=3)[N:2]([CH3:1])[C:3](=[O:24])[CH:4]=[CH:5]4)[CH:17]=[N:16][CH:15]=2)[CH2:20][CH2:19]1
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참가 물질

6

반응물 3

HCID 199401P,P-Diphenylphosphinic azideHCID 23665647Potassium tert-butoxideHCID 86679167HCID 86679167, 화합물

생성물 1

HCID 866792386-[5-(1-Amino-cyclopropyl)-pyridin-3-yl]-1-methyl-1H-quinolin-2-one수율 38.3%

시약·촉매·용매 2

HCID 1140Toluene용매
HCID 8028
Tetrahydrofuran
용매

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온도
0 °C

실험 절차

To solution of 1-(5-(1-methyl-2-oxo-1,2,3,4-tetrahydroquinolin-6-yl)pyridin-3-yl)cyclopropanecarboxylic acid (example 59 [C], 0.3 g, 0.931 mmol) in toluene (15 mL) were added TEA (0.141 g, 1.4 mmol) and diphenylphosphoryl azide (0.384 g, 1.4 mmol) and then the reaction mixture was heated to reflux for 4 h. The mixture was concentrated in vacuo, the residue was dissolved in THF (30 mL) and the solution cooled to 0° C. Then, a solution of KOtBu (0.627 g, 5.58 mmol) in THF (13 mL) was added and the mixture was stirred for 1 h at 0° C. and then over night at room temperature. The mixture was concentrated in vacuo, the residue was preadsorbed on silica gel and purified by silica gel flash chromatography eluting with a 0 to 10% MeOH-DCM gradient to give a yellow amorphous solid (0.104 g). This material was then further purified by reverse phase HPLC on a Gemini-NX column, eluting with a MeOH—H2O (0.05% TEA) gradient to give the title compound (0.02 g, 7%) as a colorless amorphous solid. MS: 292.3 (M+H+).

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 4 h
  3. concentrationThe mixture was concentrated in vacuo
  4. dissolutionthe residue was dissolved in THF (30 mL)
  5. waitover night at room temperature
  6. concentrationThe mixture was concentrated in vacuo
  7. custompurified by silica gel flash chromatography
  8. washeluting with a 0 to 10% MeOH-DCM gradient

출처 및 근거

ORD 기록
ord-3e4e895825734bf4a15f12d2df3ffde2
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09260408B2

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