Morpholine → HCID 59555451、化合物

HRID 1172231ノート

反応式

HRID 1172231 の反応式
[C:1]([C:3]1[N:8]=[C:7]([CH2:9][OH:10])[CH:6]=[CH:5][CH:4]=1)#[CH:2].[NH:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1>C(O)C>[N:11]1([CH2:2][CH2:1][C:3]2[N:8]=[C:7]([CH2:9][OH:10])[CH:6]=[CH:5][CH:4]=2)[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1

参加物

4

反応物 2

HCID 8083MorpholineHCID 56972612(6-Ethynylpyridin-2-yl)methanol

生成物 1

HCID 59555451HCID 59555451、化合物収率 22.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(6-Ethynylpyridin-2-yl)methanol (320 mg) and morpholine (1 g) were dissolved in 3 mL of ethanol, and the solution was heated to reflux under argon atmosphere for 24 hours. After allowing the reaction to cool, the ethanol was removed under reduced pressure, and the residue was basified with aqueous sodium hydroxide, and extracted with chloroform. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and the solvent was removed. The residue was purified by chromatography on silica gel (chloroform-methanol-aqueous ammonia=200:10:1) to give 122 mg of [6-(2-morpholin-4-ylethyl)pyridin-2-yl]methanol as a yellow oil.

後処理

  1. temperaturethe solution was heated
  2. temperatureto reflux under argon atmosphere for 24 hours
  3. customthe reaction
  4. temperatureto cool
  5. customthe ethanol was removed under reduced pressure
  6. extractionextracted with chloroform
  7. washThe organic layer was washed with brine
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customthe solvent was removed
  10. customThe residue was purified by chromatography on silica gel (chloroform-methanol-aqueous ammonia=200:10:1)

出典と根拠

ORDレコード
ord-7d1a4d5f75af4da093ad18ecc380f26e
出典データセット
uspto-grants-2010_11
特許番号
US07834002B2

反応ノート

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