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

Acetic Anhydride → N-[2-(1-methyl-8,9-dihydro-7H-cyclopenta[c]pyrazolo[1,5-a]pyridin-9-yl)ethyl]acetamide

HRID 887806
노트
인쇄 미리보기

반응식

HRID 887806 반응식
[NH2:1][CH2:2][CH2:3][CH:4]1[C:8]2[C:9]3[N:10]([N:13]=[CH:14][C:15]=3[C:16](OCC)=O)[CH:11]=[CH:12][C:7]=2[CH2:6][CH2:5]1.C1(C)C=CC=CC=1.[H-].C([Al+]CC(C)C)C(C)C.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].C(N(CC)CC)C.[C:62](OC(=O)C)(=[O:64])[CH3:63]>O1CCCC1.O>[CH3:16][C:15]1[CH:14]=[N:13][N:10]2[CH:11]=[CH:12][C:7]3[CH2:6][CH2:5][CH:4]([CH2:3][CH2:2][NH:1][C:62](=[O:64])[CH3:63])[C:8]=3[C:9]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 62649Sodium sulfate decahydrateHCID 59145841ethyl 9-(2-aminoethyl)-8,9-dihydro-7H-cyclopenta[c]pyrazolo[1,5-a]pyridine-1-carboxylateHCID 86583787Diisobutylaluminumhydride toluene

생성물 1

HCID 59145930
N-[2-(1-methyl-8,9-dihydro-7H-cyclopenta[c]pyrazolo[1,5-a]pyridin-9-yl)ethyl]acetamide
수율 17.2%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of ethyl 9-(2-aminoethyl)-8,9-dihydro-7H-cyclopenta[c]pyrazolo[1,5-a]pyridine-1-carboxylate (45.0 mg, 0.165 mmol) in tetrahydrofuran (1.7 mL) was added 1.5M diisobutylaluminum hydride toluene solution (1.3 mL, 1.95 mmol) at room temperature, and the mixture was stirred for 3 hr. Sodium sulfate decahydrate (1.3 g) was added, and the mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. To a mixture of the residue and triethylamine (34.5 μL, 0.248 mmol) in tetrahydrofuran (1.7 mL) was added acetic anhydride (23.4 μL, 0.248 mmol) under ice-cooling, and the mixture was stirred at room temperature for 15 min. Water (50 μL) was added, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→5/95) and recrystallization (ethyl acetate/diisopropyl ether) to give the title compound (7.3 mg, yield 17%).

후처리

  1. filtrationthe mixture was filtered through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. temperaturecooling
  4. stirringthe mixture was stirred at room temperature for 15 min
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→5/95) and recrystallization (ethyl acetate/diisopropyl ether)

출처 및 근거

ORD 기록
ord-527bec76b41c4510b91b4f3f6bbe65f0
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08247429B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트