Acetyl chloride → (S)-N-(1-(5-Hydroxypyridin-2-yl)ethyl)acetamide

HRID 40575ノート

反応式

HRID 40575 の反応式
[NH2:1][C@H:2]([C:4]1[N:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)[CH3:3].[C:11](Cl)(=[O:13])[CH3:12]>C1COCC1>[OH:10][C:7]1[CH:6]=[CH:5][C:4]([C@@H:2]([NH:1][C:11](=[O:13])[CH3:12])[CH3:3])=[N:9][CH:8]=1

参加物

4

実験手順

To 1.00 g (5.73 mmol) (S)-6-(1-aminoethyl)pyridin-3-ol in 10 ml THF and 3.99 mL TEA (28.6 mmol) are slowly added 494 mg (6.30 mmol) acetyl chloride and stirring is continued for 2 h. The reaction is quenched by the addition of water and extracted several times with DCM. The org. layers are combined, dried over MgSO4, filtered and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, DCM/MeOH/NH3 90/9/1).

後処理

  1. customThe reaction is quenched by the addition of water
  2. extractionextracted several times with DCM
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customthe solvent is removed in vacuo
  6. customThe crude product is purified by column chromatography (silica gel, DCM/MeOH/NH3 90/9/1)

出典と根拠

ORDレコード
ord-e05a20423a9346b1b6c342b34195757b
出典データセット
uspto-grants-2013_09
特許番号
US08530460B2

反応ノート

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