Imidazole → HCID 178455364、化合物

HRID 1243163ノート

反応式

HRID 1243163 の反応式
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([OH:8])[CH2:4][CH2:3]1.N1C=CN=C1.[Si:14](Cl)([C:17]([CH3:20])([CH3:19])[CH3:18])([CH3:16])[CH3:15]>ClCCl>[C:17]([Si:14]([CH3:16])([CH3:15])[O:8][C@H:5]1[CH2:6][CH2:7][C@H:2]([NH2:1])[CH2:3][CH2:4]1)([CH3:20])([CH3:19])[CH3:18]

参加物

5

反応物 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 178511715HCID 178511715、化合物

生成物 1

HCID 178455364HCID 178455364、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of trans-4-aminocyclohexanol (5.0 g, 43.4 mmol) (TCl US) in dichloromethane (100 mL) was added imidazole (14.78 g, 0.22 mol) (Aldrich) and tert-butyldimethylsilyl chloride (19.63 g, 0.13 mol) (Avocardo Research Chemicals). The reaction mixture was stirred at room temperature for 1 day and then was concentrated under reduced pressure. The residue was partitioned between ethyl acetate (100 mL) and water (100 mL). The organic layer was washed with 1N sodium hydroxide solution, water and brine, dried over magnesium sulfate, filtered and concentrated to give trans-4-(tert-butyl-dimethyl-silanyloxy)-cyclohexylamine. (Yield 7.62 g, 76.5%).

後処理

  1. concentrationwas concentrated under reduced pressure
  2. customThe residue was partitioned between ethyl acetate (100 mL) and water (100 mL)
  3. washThe organic layer was washed with 1N sodium hydroxide solution, water and brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-b69c894cac4b45f49c3c7acddad21308
出典データセット
uspto-grants-2006_10
特許番号
US07115740B2

反応ノート

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