Hexane → HCID 69423031、化合物

HRID 349897ノート

反応式

HRID 349897 の反応式
[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

参加物

6

反応物 4

HCID 8058HexaneHCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23024929HCID 23024929、化合物

生成物 1

HCID 69423031HCID 69423031、化合物収率 95.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-7c5706f830504338b095d525a8ce0598
出典データセット
uspto-grants-2007_02
特許番号
US07179823B1

反応ノート

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