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Water → pentyl[2'-(1-trityl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]amine

HRID 492294
ノート
印刷プレビュー

反応式

HRID 492294 の反応式
[C:1]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]2[N:25]([C:26]([C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[N:24]=[N:23][N:22]=2)=[CH:11][CH:10]=1)(=O)[CH2:2][CH2:3][CH2:4][CH3:5].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH2:1]([NH:7][CH2:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]2[N:25]([C:26]([C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=3)([C:39]3[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=3)[C:33]3[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=3)[N:24]=[N:23][N:22]=2)=[CH:13][CH:14]=1)[CH2:2][CH2:3][CH2:4][CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 23569449N-[[2'-(1-Trityl-1H-tetrazol-5-yl)biphenyl-4-yl]methyl] Pentanamide

生成物 1

HCID 19024425pentyl[2'-(1-trityl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]amine収率 100%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

N-Pentanoyl-N-[[2′-[N-(triphenylmethyl)tetrazol-5-yl]-1,1′-biphenyl-4-yl]methyl]amine (1.61 g) was dissolved in tetrahydrofuran (40 mL) and at room temperature, lithium aluminum hydride (340.1 mg) was added, and then the mixture was heated under reflux. Ninety minutes later, water (5 mL), a 10% aqueous solution of sodium hydroxide (5 mL) and water (5 mL) were added successively under ice bath cooling. The organic layer was separated, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. As water remained to the residue, ethyl acetate was added to conduct extraction twice from the remaining water. The organic layer was dried over anhydrous sodium sulfate, and then concentrated under reduced pressure to afford N-pentyl-N-[[2′-[N-(triphenylmethyl)tetrazol-5-yl]-1,1′-biphenyl-4-yl]methyl] amine (1.57 g). Yield: 100%.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. temperaturecooling
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionwas added
  8. extractionextraction twice from the remaining water
  9. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  10. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-558e713334c34a8ca569e6e212f7b1b1
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531576B2

反応ノート

読み込み中…

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