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

Lithium hydroxide, monohydrate → 6-[4-Methoxy-2-methyl-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboxylic acid

HRID 873519
노트
인쇄 미리보기

반응식

HRID 873519 반응식
O.[OH-].[Li+].[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:17]=[C:16]([C:18]([O:20]C)=[O:19])[CH:15]=[CH:14][CH:13]=2)=[C:8]([CH3:22])[C:7]=1[CH:23]1[C:36]2[C:35](=[O:37])[CH2:34][C:33]([CH3:39])([CH3:38])[CH2:32][C:31]=2[O:30][C:29]2[CH2:28][C:27]([CH3:41])([CH3:40])[CH2:26][C:25](=[O:42])[C:24]1=2>O.C1COCC1>[CH3:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:17]=[C:16]([C:18]([OH:20])=[O:19])[CH:15]=[CH:14][CH:13]=2)=[C:8]([CH3:22])[C:7]=1[CH:23]1[C:24]2[C:25](=[O:42])[CH2:26][C:27]([CH3:40])([CH3:41])[CH2:28][C:29]=2[O:30][C:31]2[CH2:32][C:33]([CH3:39])([CH3:38])[CH2:34][C:35](=[O:37])[C:36]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 117700765Methyl 6-[4-methoxy-2-methyl-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboxylate

생성물 1

HCID 1177005176-[4-Methoxy-2-methyl-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboxylic acid수율 73.5%

시약·촉매·용매 2

HCID 962Water용매
2회
HCID 8028Tetrahydrofuran용매

실험 절차

A solution of lithium hydroxide monohydrate (0.18 g, 4.36 mmol) in water (10.5 ml) was added dropwise to a solution of the methyl 6-[4-methoxy-2-methyl-3-(3,3,6,6-tetramethyl-1,8-dioxo-2,3,4,5,6,7,8,9-octahydro-1H-xanthen-9-yl)phenyl]pyridine-2-carboxylate produced in Example 4-3 (1.05 g, 1.98 mmol) in THF (21 ml) at room temperature, and the mixture thus obtained was then stirred at the same temperature as above for 3 hours. Thereafter, water was added to the reaction solution, and the mixed solution was then washed with diethyl ether. Thereafter, a 1 N aqueous solution of hydrochloric acid (4.36 ml) was added to the water layer, and the mixed solution was then extracted with dichloromethane. The organic layer thus obtained was dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure, and the residue thus obtained was then washed with a mixed solution of diethyl ether and hexane, followed by collection by filtration and drying, to obtain the title compound (0.75 g, yield: 73%).

후처리

  1. customthe mixture thus obtained
  2. washthe mixed solution was then washed with diethyl ether
  3. additionThereafter, a 1 N aqueous solution of hydrochloric acid (4.36 ml) was added to the water layer
  4. extractionthe mixed solution was then extracted with dichloromethane
  5. customThe organic layer thus obtained
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled away under reduced pressure
  8. customthe residue thus obtained
  9. washwas then washed with a mixed solution of diethyl ether and hexane
  10. filtrationfollowed by collection by filtration
  11. customdrying

출처 및 근거

ORD 기록
ord-181f711c211b4f17a4409227fb8fbb0d
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08975263B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트