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Acetic Acid → HCID 53657667, 화합물

HRID 1699625
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인쇄 미리보기

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HRID 1699625 반응식
C(O)(=O)C.[N:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH2:11][NH:12][C:13](=[O:35])[C:14]1[CH:19]=[CH:18][C:17]([NH:20][C:21](=O)[CH3:22])=[C:16]([NH:24][CH2:25][C:26]2[CH:31]=[CH:30][C:29]3[O:32][CH2:33][O:34][C:28]=3[CH:27]=2)[CH:15]=1>C(O)C>[CH3:22][C:21]1[N:24]([CH2:25][C:26]2[CH:31]=[CH:30][C:29]3[O:32][CH2:33][O:34][C:28]=3[CH:27]=2)[C:16]2[CH:15]=[C:14]([C:13](=[O:35])[NH:12][CH2:11][C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][N:5]=3)[CH:19]=[CH:18][C:17]=2[N:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 18315487HCID 18315487, 화합물

생성물 1

HCID 53657667HCID 53657667, 화합물수율 57.6%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
70 °C

실험 절차

Acetic acid (2 ml) and ethanol (5 ml) are added to an N-(2-pyridylmethyl)-4-acetylamino-3-(3,4-methylenedioxybenzylamino)benzamide (0.490 g) and the solution is stirred for eight hours at 70° C. The residue obtained by reduced pressure condensation is purified using silica gel column chromatography (eluate: ethyl acetate/methanol=9/1), and crystallization is performed in ethyl acetate. The crystals are separated through filtration, dried and thus, 2-methyl-1-(3,4-methylenedioxybenzyl)-6-[(2-pyridylmethyl)carbamoyl]benzimidazole (0.270 g) is obtained. 1H-NMR (CDCl3, δ): 2.59 (3H, s), 4.78 (2H, d, J=4.8 Hz), 5.28 (2H, s), 5.93 (2H, s), 6.51 (1H, d, J=1.6 Hz), 6.55 (1H, dd, J=1.4 and 7.9 Hz), 6.72 (2H, d, J=8.0 Hz), 7.22 (1H, dd, J=6.7 and 5.0 Hz), 7.34 (1H, d, J=7.7 Hz), 7.62 (1H, br t), 7.67-7.75 (3H, m), 7.96 (1H, d, J=1.1 Hz), 8.58 (1H, d, J=4.9 Hz).

후처리

  1. customThe residue obtained by reduced pressure condensation
  2. customis purified
  3. customsilica gel column chromatography (eluate: ethyl acetate/methanol=9/1), and crystallization
  4. customThe crystals are separated through filtration
  5. customdried

출처 및 근거

ORD 기록
ord-cf0bab68a44d4e03a121ef67d7d161bc
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06348032B1

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