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

1,1,1-Trimethoxybutane → ethyl 4-(5,6-dimethyl-8-propyl-7H-imidazo[4,5-c]tetraazolo[1,5-a]pyridin-7-yl)butanoate

HRID 2366703
노트
인쇄 미리보기

반응식

HRID 2366703 반응식
Cl.N1C=[CH:6][CH:5]=[CH:4][CH:3]=1.C(OC)(OC)(OC)CCC.[NH2:18][C:19]1[C:20]2[N:21]([N:36]=[N:37][N:38]=2)[C:22]([CH3:35])=[C:23]([CH3:34])[C:24]=1[NH:25][CH2:26][CH2:27][CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30]>C1(C)C=CC=CC=1>[CH3:35][C:22]1[N:21]2[N:36]=[N:37][N:38]=[C:20]2[C:19]2[N:18]=[C:3]([CH2:4][CH2:5][CH3:6])[N:25]([CH2:26][CH2:27][CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])[C:24]=2[C:23]=1[CH3:34]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1235121,1,1-TrimethoxybutaneHCID 10176127Pyridinium chlorideHCID 57447079Ethyl 4-[(8-amino-5,6-dimethyltetraazolo[1,5-a]pyridin-7-yl)amino]butanoate

생성물 1

HCID 69506777ethyl 4-(5,6-dimethyl-8-propyl-7H-imidazo[4,5-c]tetraazolo[1,5-a]pyridin-7-yl)butanoate수율 150.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

For Examples 40 and 41, pyridine hydrochloride (1.34 g, 11.6 mmol) and trimethyl orthobutyrate (5.42 mL, 34.1 mmol) were sequentially added with stirring to a solution of ethyl 4-[(8-amino-5,6-dimethyltetraazolo[1,5-a]pyridin-7-yl)amino]butanoate (9.1 g, 31 mmol) in toluene (310 mL) under a nitrogen atmosphere. The reaction was heated at reflux for 1.5 hours, allowed to cool to ambient temperature overnight, and concentrated under reduced pressure. The residue was partitioned between chloroform (300 mL) and saturated aqueous sodium bicarbonate (75 mL). The aqueous layer was extracted with chloroform (2×100 mL), and the combined organic fractions were washed with saturated aqueous sodium bicarbonate (2×75 mL), dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The resulting solid was triturated with ethyl acetate and isolated by filtration to provide 6.0 g of ethyl 4-(5,6-dimethyl-8-propyl-7H-imidazo[4,5-c]tetraazolo[1,5-a]pyridin-7-yl)butanoate as a white solid.

후처리

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 1.5 hours
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was partitioned between chloroform (300 mL) and saturated aqueous sodium bicarbonate (75 mL)
  5. extractionThe aqueous layer was extracted with chloroform (2×100 mL)
  6. washthe combined organic fractions were washed with saturated aqueous sodium bicarbonate (2×75 mL)
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe resulting solid was triturated with ethyl acetate
  11. customisolated by filtration

출처 및 근거

ORD 기록
ord-ee442391adbd4cc0ab6dcb9db7351fbe
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697873B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트