Acetic Acid → 3-(1-Benzyl-2-oxo-2,5,6,7-tetrahydro-1h-azepin-3-yl)-n-hydroxy-propionamide

HRID 2240614노트

반응식

HRID 2240614 반응식
C[O:2][C:3](=O)[CH2:4][CH2:5][C:6]1[C:7](=[O:20])[N:8]([CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:9][CH2:10][CH2:11][CH:12]=1.CO.[NH2:24][O:25][K].C(O)(=O)C>C(OCC)(=O)C>[CH2:13]([N:8]1[CH2:9][CH2:10][CH2:11][CH:12]=[C:6]([CH2:5][CH2:4][C:3]([NH:24][OH:25])=[O:2])[C:7]1=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 887MethanolHCID 685828973-(1-Benzyl-2-oxo-2,5,6,7-tetrahydro-1H-azepin-3-yl)-propionic acid methyl esterHCID 178514655HCID 178514655, 화합물

생성물 1

HCID 112547463-(1-Benzyl-2-oxo-2,5,6,7-tetrahydro-1h-azepin-3-yl)-n-hydroxy-propionamide수율 43%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

108 mg of compound (d) prepared by the above Step 3 was dissolved in methanol solution (0.376 mmol) and then 1.7 M methanolic suspension solution containing NH2OK (1.315 ml, 2.63 mmol) 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 46 mg of the title compound (e1) (yield: 43%).

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-1ff50168c45043a893448831e28cf43d
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723376B2

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