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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triethylamine → 1,1-Dimethylethyl (2S)-4-({6-[({6-[(4-fluorophenyl)oxy]-3-pyridinyl}carbonyl)(methyl)amino]-4-methyl-3-pyridinyl}methyl)-2-methyl-1-piperazinecarboxylate

HRID 534788
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HRID 534788 반응식
[CH3:1][C@H:2]1[CH2:7][N:6]([CH2:8][C:9]2[CH:10]=[N:11][C:12]([NH:16][CH3:17])=[CH:13][C:14]=2[CH3:15])[CH2:5][CH2:4][N:3]1[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19].C(N(CC)CC)C.[F:32][C:33]1[CH:38]=[CH:37][C:36]([O:39][C:40]2[N:45]=[CH:44][C:43]([C:46](Cl)=[O:47])=[CH:42][CH:41]=2)=[CH:35][CH:34]=1.C([O-])(O)=O.[Na+]>C(Cl)Cl>[F:32][C:33]1[CH:38]=[CH:37][C:36]([O:39][C:40]2[N:45]=[CH:44][C:43]([C:46]([N:16]([CH3:17])[C:12]3[N:11]=[CH:10][C:9]([CH2:8][N:6]4[CH2:5][CH2:4][N:3]([C:18]([O:20][C:21]([CH3:22])([CH3:24])[CH3:23])=[O:19])[C@@H:2]([CH3:1])[CH2:7]4)=[C:14]([CH3:15])[CH:13]=3)=[O:47])=[CH:42][CH:41]=2)=[CH:35][CH:34]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 231490426-[(4-Fluorophenyl)oxy]-3-pyridinecarbonyl chlorideHCID 592621971,1-Dimethylethyl (2S)-2-methyl-4-{[4-methyl-6-(methylamino)-3-pyridinyl]methyl}-1-piperazinecarboxylate

생성물 1

HCID 592621991,1-Dimethylethyl (2S)-4-({6-[({6-[(4-fluorophenyl)oxy]-3-pyridinyl}carbonyl)(methyl)amino]-4-methyl-3-pyridinyl}methyl)-2-methyl-1-piperazinecarboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

1,1-Dimethylethyl (2S)-2-methyl-4-{[4-methyl-6-(methylamino)-3-pyridinyl]methyl}-1-piperazinecarboxylate (D101) (0.038 g, 0.11 mmol) was dissolved in dry DCM (2 mL). Triethylamine (0.016 g, 0.16 mmol) was added dropwise and after 5 minutes a solution of the acid chloride from step 1 in dry DCM (2 mL) was added dropwise. The reaction mixture was then left stirring under argon at room temperature overnight. Saturated aqueous NaHCO3 (15 mL) was added and the aqueous layer extracted with DCM (3×5 mL). The organic extracts were dried (Na2SO4) and the crude product was purified by column chromatography. Elution with a 0-100% EtOAc/petroleum ether gradient gave the title compound as a colourless oil (0.026 g). MS (ES): MH+ 550.4

후처리

  1. additionwas added dropwise
  2. waitThe reaction mixture was then left
  3. extractionthe aqueous layer extracted with DCM (3×5 mL)
  4. dry with materialThe organic extracts were dried (Na2SO4)
  5. customthe crude product was purified by column chromatography
  6. washElution with a 0-100% EtOAc/petroleum ether gradient

출처 및 근거

ORD 기록
ord-c3126446feba4cbda58f77307a244f81
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853218B2

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