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Acetic Acid → 1,2,5,6-Tetrahydro-N-hydroxy-1-methyl-2-oxo-3-pyridinepropanamide

HRID 2240611
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HRID 2240611 반응식
C[O:2][C:3](=O)[CH2:4][CH2:5][C:6]1[C:7](=[O:13])[N:8]([CH3:12])[CH2:9][CH2:10][CH:11]=1.[NH2:15][O:16][K].C(O)(=O)C>CO.C(OCC)(=O)C>[OH:16][NH:15][C:3](=[O:2])[CH2:4][CH2:5][C:6]1[C:7](=[O:13])[N:8]([CH3:12])[CH2:9][CH2:10][CH:11]=1
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참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 16720334HCID 16720334, 화합물HCID 178514655HCID 178514655, 화합물

생성물 1

HCID 114129481,2,5,6-Tetrahydro-N-hydroxy-1-methyl-2-oxo-3-pyridinepropanamide수율 35%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 8857Ethyl Acetate
용매

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온도
0 °C

실험 절차

50 mg of 3-(1-methyl-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl)-propionic acid methyl ester prepared from the above Step 1 was dissolved in methanol (0.25 mM) and then 0.122 ml of 1.7M NH2OK suspension solution in methanol (0.207 mM) was added thereto at 0° C. and the resulting mixture was 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, filtered and concentrated in vacuo. The resulting compound was purified by column chromatography on Silica gel with methanol/chloroform (1:20) solvent mixture as an eluant to give 19 mg of the title compound (j2) (yield: 35%).

후처리

  1. filtrationfiltered
  2. concentrationconcentrated in vacuo
  3. customThe resulting compound was purified by column chromatography on Silica gel with methanol/chloroform (1:20) solvent mixture as an eluant

출처 및 근거

ORD 기록
ord-5077e34e76a2477fa6fdb510c5f28b8e
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07723376B2

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