Methanol → 9-Chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide

HRID 2212192

반응식

HRID 2212192 반응식
[I:1][Si](C)(C)C.COC([N:10]1[CH2:15][CH2:14][CH2:13][CH:12]([N:16]2[C:25]3[CH:24]=[CH:23][CH:22]=[C:21]([Cl:26])[C:20]=3[C:19]3=[N:27][O:28][C:29]([CH3:30])=[C:18]3[C:17]2=[O:31])[CH2:11]1)=O.CO.C(OCC)C>ClCCl>[IH:1].[Cl:26][C:21]1[C:20]2[C:19]3[C:18](=[C:29]([CH3:30])[O:28][N:27]=3)[C:17](=[O:31])[N:16]([CH:12]3[CH2:13][CH2:14][CH2:15][NH:10][CH2:11]3)[C:25]=2[CH:24]=[CH:23][CH:22]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 3283Diethyl EtherHCID 85247Trimethylsilyl iodideHCID 99515613-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidine-1-carboxylic acid methyl ester

생성물 1

HCID 219637129-Chloro-3-methyl-5-piperidin-3-yl-5H-isoxazolo[4,3-c]quinolin-4-one hydroiodide수율 97%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Add iodotrimethylsilane (1.87 mL, 13.16 mmol) to a solution of 3-(9-chloro-3-methyl-4-oxo-5H-isoxazolo[4,3-c]quinolin-5-yl)-piperidine-1-carboxylic acid methyl ester (2.06 g, 5.48 mmol) in dichloromethane (40 mL). Stir the solution at room temperature under nitrogen overnight. Add methanol (3.2 mL, 78.93 mmol) dropwise, and stir the reaction at room temperature for 30 minutes. Concentrate the reaction, add to diethyl ether, sonicate, and filtere. Dry the solids on a vacuum pump to give 2.36 g of the title compound as a tan solid, 97% yield. 1H NMR: consistent with structure. MS (ion spray) 318 (M+).

후처리

  1. customthe reaction at room temperature for 30 minutes
  2. concentrationConcentrate
  3. customthe reaction
  4. customsonicate
  5. customDry the solids on a vacuum pump

출처 및 근거

ORD 기록
ord-769fcdf1cdd8433c89c93ffe0bcf8a88
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07101891B2

연결된 노트

불러오는 중…