Acetic Acid → HCID 11276149, 화합물

HRID 2240609노트

반응식

HRID 2240609 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

HCID 11276149HCID 11276149, 화합물수율 48%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5cb32b194c12456da4e597e80b663639
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723376B2

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