Acetic Acid → 3-[1-(2,4-Dimethoxybenzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl]-n-hydroxy-propionamide

HRID 2240595노트

반응식

HRID 2240595 반응식
C[O:2][C:3](=O)[CH2:4][CH2:5][C:6]1[C:7](=[O:23])[N:8]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]=2[O:21][CH3:22])[CH2:9][CH2:10][CH:11]=1.[NH2:25][O:26][K].C(O)(=O)C>CO.C(OCC)(=O)C>[CH3:22][O:21][C:14]1[CH:15]=[C:16]([O:19][CH3:20])[CH:17]=[CH:18][C:13]=1[CH2:12][N:8]1[CH2:9][CH2:10][CH:11]=[C:6]([CH2:5][CH2:4][C:3]([NH:25][OH:26])=[O:2])[C:7]1=[O:23]

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 16720333HCID 16720333, 화합물HCID 178514655HCID 178514655, 화합물

생성물 1

HCID 113020733-[1-(2,4-Dimethoxybenzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl]-n-hydroxy-propionamide수율 73%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

46 mg of compound (d) prepared by the above Step 3 was dissolved in methanol solution (0.138 mM) and then 1.7 M methanolic suspension solution containing NH2OK (0.122 ml, 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 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 32 mg of the title compound (e1) (yield: 73%).

후처리

  1. additionwas added
  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-23a1241b1a1f404ead9b6d3a2780f596
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723376B2

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