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

HRID 588049노트

반응식

HRID 588049 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-073a09ed8562437cbf4ede7277124b43
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227955B2

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