Sodium sulfate decahydrate → [1-[6-(5-Methyl-2-phenyl-4-oxazolylmethoxy)-3-pyridylmethyl]-4-phenyl-3-pyrrolyl]methanol

HRID 349994

反応式

HRID 349994 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[N:26]=[CH:25][C:24]([CH2:27][N:28]2[CH:32]=[C:31]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:30]([C:39](OC)=[O:40])=[CH:29]2)=[CH:23][CH:22]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>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[N:26]=[CH:25][C:24]([CH2:27][N:28]2[CH:32]=[C:31]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:30]([CH2:39][OH:40])=[CH:29]2)=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 69423340Methyl 1-[6-(5-methyl-2-phenyl-4-oxazolylmethoxy)-3-pyridylmethyl]-4-phenylpyrrole-3-carboxylate

生成物 1

HCID 69422752[1-[6-(5-Methyl-2-phenyl-4-oxazolylmethoxy)-3-pyridylmethyl]-4-phenyl-3-pyrrolyl]methanol収率 94%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium aluminium hydride (205 mg) was added gradually to a solution of methyl 1-[6-(5-methyl-2-phenyl-4-oxazolylmethoxy)-3-pyridylmethyl]-4-phenylpyrrole-3-carboxylate (1.30 g) in tetrahydrofuran (40 ml) at 0° C., and the resultant was stirred for 3 hours. Sodium sulfate decahydrate (2.80 g) was added to the reaction mixture, and the precipitate was removed by filtration. The filtrate was concentrated, and the residue was subjected to silica gel column chromatography to obtain [1-[6-(5-methyl-2-phenyl-4-oxazolylmethoxy)-3-pyridylmethyl]-4-phenyl-3-pyrrolyl]methanol (1.15 g, yield 94%) as a colorless oily substance from the fraction eluted with ethyl acetate-hexane (3:2, volume ratio).

後処理

  1. customthe precipitate was removed by filtration
  2. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-464073a1055e4e83b01ab7735a14d550
出典データセット
uspto-grants-2007_02
特許番号
US07179823B1

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