Acetic Acid → HCID 11276149、化合物

HRID 2240609ノート

反応式

HRID 2240609 の反応式
C[O:2][C:3](=O)[CH2:4][CH2:5][C:6]1[C:7](=[O:15])[N:8]([CH2:12][CH:13]=[CH2:14])[CH2:9][CH2:10][CH:11]=1.[NH2:17][O:18][K].C(O)(=O)C>CO.C(OCC)(=O)C>[CH2:12]([N:8]1[CH2:9][CH2:10][CH:11]=[C:6]([CH2:5][CH2:4][C:3]([NH:17][OH:18])=[O:2])[C:7]1=[O:15])[CH:13]=[CH2:14]

参加物

6

反応物 3

HCID 176Acetic AcidHCID 167205483-(1-Allyl-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid methyl esterHCID 178514655HCID 178514655、化合物

生成物 1

HCID 11276149HCID 11276149、化合物収率 48%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

24 mg of 3-(1-allyl-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid methyl ester (i1) prepared from the above Step 2 was dissolved in methanol solution (0.11 mM) and then 0.122 ml of 1.7M NH2OK suspension solution (0.207 mM) was added thereto at 0° c. and stirred for 3 hrs at room temperature. The resulting mixture was neutralized with 0.02 ml of acetic acid, diluted with 10 ml of ethyl acetate solution, filtered and concentrated in vacuo. The resulting compound was purified by column chromatography on Silica gel with methanol/chloroform (1:10) solvent mixture as an eluant to give 11 mg of the title compound (j1) (yield: 48%).

後処理

  1. customat 0°
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. customThe resulting compound was purified by column chromatography on Silica gel with methanol/chloroform (1:10) solvent mixture as an eluant

出典と根拠

ORDレコード
ord-5cb32b194c12456da4e597e80b663639
出典データセット
uspto-grants-2010_05
特許番号
US07723376B2

反応ノート

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