Hydrochloric Acid → 2-(Propan-2-yl)morpholine

HRID 737108노트

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HRID 737108 반응식
C(OC([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH:14]([CH3:16])[CH3:15])[CH2:9]1)=O)(C)(C)C.Cl>O1CCOCC1>[CH:14]([CH:10]1[O:11][CH2:12][CH2:13][NH:8][CH2:9]1)([CH3:16])[CH3:15]

참가 물질

4

실험 절차

The above compound could be made in the following manner: 2-Isopropyl-morpholine-4-carboxylic acid tert-butyl ester in 4N solution of hydrogen chloride in dioxane could be stirred at 60° C. for 3 h. The solvent could be removed in vacuo and 1N aqueous hydrogen chloride solution could be added to the resulting residue, and the mixture could be washed with diethyl ether. The aqueous layer could be adjusted to pH 14 by addition of 2N NaOH solution and extracted with methylene chloride. The organic layer could be washed with brine and dried over sodium sulfate. After filtering, the material could be purified by column chromatography.

후처리

  1. customThe solvent could be removed in vacuo and 1N aqueous hydrogen chloride solution
  2. additioncould be added to the resulting residue
  3. washthe mixture could be washed with diethyl ether
  4. additionThe aqueous layer could be adjusted to pH 14 by addition of 2N NaOH solution
  5. extractionextracted with methylene chloride
  6. washThe organic layer could be washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationAfter filtering
  9. customthe material could be purified by column chromatography

출처 및 근거

ORD 기록
ord-afa4af7f1e1c4be7a55aee4bbb368bba
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07595397B2

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