Hexane → HCID 69423031, 화합물

HRID 349897노트

반응식

HRID 349897 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[O:12][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:10][C:9]=1[CH2:19][O:20][C:21]1[CH:43]=[CH:42][C:24]([CH2:25][N:26]2[CH:30]=[C:29]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][N:32]=3)[C:28]([C:37](OCC)=[O:38])=[CH:27]2)=[CH:23][CH:22]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].CCCCCC>O1CCCC1>[CH3:7][C:8]1[O:12][C:11]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)=[N:10][C:9]=1[CH2:19][O:20][C:21]1[CH:22]=[CH:23][C:24]([CH2:25][N:26]2[CH:30]=[C:29]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][N:32]=3)[C:28]([CH2:37][OH:38])=[CH:27]2)=[CH:42][CH:43]=1

참가 물질

6

반응물 4

HCID 8058HexaneHCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23024929HCID 23024929, 화합물

생성물 1

HCID 69423031HCID 69423031, 화합물수율 95.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Lithium aluminium hydride (0.25 g) was added to a solution of ethyl 1-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl]-4-(2-pyridyl)pyrrole-3-carboxylate (2.40 g) in tetrahydrofuran (30 ml) at 0° C., and the mixture was stirred at 0° C. for 30 minutes. After sodium sulfate decahydrate (2.13 g) and hexane (30 ml) were added to the reaction mixture, the mixture was stirred at room temperature for 30 minutes. After the precipitate was removed by filtration, the filtrate was concentrated. The residue was subjected to silica gel column chromatography, and [1-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl]-4-(2-pyridyl)-3-pyrrolyl]methanol (2.09 g, yield: 95%) was obtained as an oily substance from the fraction eluted with ethyl acetate-hexane (1:1, volume ratio).

후처리

  1. stirringthe mixture was stirred at room temperature for 30 minutes
  2. customAfter the precipitate was removed by filtration
  3. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-7c5706f830504338b095d525a8ce0598
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179823B1

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