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Methane → tert-butyl 2-{2-[2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethylcarbamate

HRID 719215
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인쇄 미리보기

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HRID 719215 반응식
[NH2:1][C:2]1[CH:3]=[N:4][C:5]2[C:10]([C:11]=1[NH:12][CH2:13][CH2:14][O:15][CH2:16][CH2:17][NH:18][C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:9][CH:8]=[CH:7][CH:6]=2.C(N(CC)CC)C.[CH3:33][O:34][CH2:35][CH2:36][C:37](Cl)=O.C>C(Cl)Cl.CCO.CO>[CH3:33][O:34][CH2:35][CH2:36][C:37]1[N:12]([CH2:13][CH2:14][O:15][CH2:16][CH2:17][NH:18][C:19](=[O:25])[O:20][C:21]([CH3:22])([CH3:24])[CH3:23])[C:11]2[C:10]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=3[N:4]=[CH:3][C:2]=2[N:1]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 297MethaneHCID 8471Triethylamine2회HCID 27597283-Methoxypropanoyl chlorideHCID 12106200Tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy)ethylcarbamate

생성물 1

HCID 12106201tert-butyl 2-{2-[2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethylcarbamate수율 90.8%

시약·촉매·용매 3

HCID 702
Ethanol
용매
HCID 887Methanol용매
HCID 6344Dichloromethane용매

실험 절차

A solution of tert-butyl 2-{2-[(3-aminoquinolin-4-yl)amino]ethoxy}ethylcarbamate (10.2 g, 29.5 mmol) in 250 mL of anhydrous CH2Cl2 was cooled to 0° C. and treated with triethylamine (4.18 mL, 30.0 mmol). Methoxypropionyl chloride (3.30 mL, 30.3 mmol) was then added dropwise over 5 min. The reaction was then warmed to room temperature and stirring was continued for 1 h. The reaction mixture was then concentrated under reduced pressure to give an orange solid. This was dissolved in 250 mL of EtOH and 12.5 mL of triethylamine was added. The mixture was heated to reflux and stirred under N2 overnight. The reaction was then concentrated to dryness under reduced pressure and treated with 300 mL of Et2O. The mixture was then filtered and the filtrate was concentrated under reduced pressure to give a brown solid. The solid was dissolved in 200 mL of hot MeOH and treated with activated charcoal. The hot solution was filtered and concentrated to give 11.1 g of tert-butyl 2-{2-[2-(2-methoxyethyl)-1H-imidazo[4,5-c]quinolin-1-yl]ethoxy}ethylcarbamate as a yellow syrup.

후처리

  1. concentrationThe reaction mixture was then concentrated under reduced pressure
  2. customto give an orange solid
  3. temperatureThe mixture was heated
  4. temperatureto reflux
  5. stirringstirred under N2 overnight
  6. concentrationThe reaction was then concentrated to dryness under reduced pressure
  7. additiontreated with 300 mL of Et2O
  8. filtrationThe mixture was then filtered
  9. concentrationthe filtrate was concentrated under reduced pressure
  10. customto give a brown solid
  11. filtrationThe hot solution was filtered
  12. concentrationconcentrated

출처 및 근거

ORD 기록
ord-6dbae68bc0db4420aa60af450d91b325
출처 데이터셋
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07132429B2

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