Hydrochloric Acid → 2-(4-Aminopiperidin-1-yl)ethan-1-ol

HRID 588049ノート

反応式

HRID 588049 の反応式
[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][CH:7]([NH:10]C(=O)OC(C)(C)C)[CH2:6][CH2:5]1.Cl>C(O)C>[NH2:10][CH:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][OH:1])[CH2:5][CH2:6]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 45076484[1-(2-Hydroxy-ethyl)-piperidin-4-yl]-carbamic acid tert-butyl ester

生成物 1

HCID 157334452-(4-Aminopiperidin-1-yl)ethan-1-ol収率 96.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 0.58 g of tert-butyl 1-(2-hydroxyethyl)piperidin-4-ylcarbamate obtained in step 1 in 10 ml of ethanol was added 1 ml of conc. HCl, followed by stirring for 2 hrs under reflux. The reaction mixture was cooled to room temperature, and concentrated in a reduced pressure to remove solvent. The residue was added with 10 ml of distilled water, neutralized with saturated sodium hydrogen carbonate aqueous solution, and extracted twice with 10 ml of methylene chloride. After being dried over a desiccant, the fraction was concentrated in a reduced pressure to afford 0.33 g of the title compound (Yield: 95%). 1H NMR (CDCl3) δ 3.68 (s, 2H), 3.60 (t, 2H), 2.86 (d, 2H), 2.69 (m, 1H), 2.53 (t, 2H), 2.11 (t, 2H), 1.82 (d, 2H), 1.42 (t, 2H) ppm.

後処理

  1. temperatureunder reflux
  2. concentrationconcentrated in a reduced pressure
  3. customto remove solvent
  4. additionThe residue was added with 10 ml of distilled water
  5. extractionextracted twice with 10 ml of methylene chloride
  6. customAfter being dried over a desiccant, the fraction
  7. concentrationwas concentrated in a reduced pressure

出典と根拠

ORDレコード
ord-073a09ed8562437cbf4ede7277124b43
出典データセット
uspto-grants-2016_01
特許番号
US09227955B2

反応ノート

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