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

HRID 737108ノート

反応式

HRID 737108 の反応式
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]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57849505HCID 57849505、化合物

生成物 1

HCID 198776882-(Propan-2-yl)morpholine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-afa4af7f1e1c4be7a55aee4bbb368bba
出典データセット
uspto-grants-2009_09
特許番号
US07595397B2

反応ノート

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