9-(1-benzyl-4-methyl-1H-imidazol-2-yl)-8-phenyl-8,9-dihydro-2H-pyrido[4,3,2-de]phthalazin-3(7H)-one → HCID 178430837, 화합물

HRID 907851노트

반응식

HRID 907851 반응식
C([N:8]1[CH:12]=[C:11]([CH3:13])[N:10]=[C:9]1[CH:14]1[C:19]2=[N:20][NH:21][C:22](=[O:27])[C:23]3[CH:24]=[CH:25][CH:26]=[C:17]([C:18]=32)[NH:16][CH:15]1[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)C1C=CC=CC=1>[OH-].[OH-].[Pd+2].CO>[CH3:13][C:11]1[N:10]=[C:9]([CH:14]2[C:19]3=[N:20][NH:21][C:22](=[O:27])[C:23]4[CH:24]=[CH:25][CH:26]=[C:17]([C:18]=43)[NH:16][CH:15]2[C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[NH:8][CH:12]=1

참가 물질

4

반응물 1

HCID 1363747039-(1-benzyl-4-methyl-1H-imidazol-2-yl)-8-phenyl-8,9-dihydro-2H-pyrido[4,3,2-de]phthalazin-3(7H)-one

생성물 1

HCID 178430837HCID 178430837, 화합물수율 87.4%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 887Methanol용매

실험 절차

A mixture of 9-(1-benzyl-4-methyl-1H-imidazol-2-yl)-8-phenyl-8,9-dihydro-2H-pyrido[4,3,2-de]phthalazin-3(7H)-one (40 mg, 0.09 mmol) and palladium hydroxide on carbon catalyst (40 mg, 20% wt) in anhydrous methanol (15 mL) was purged with hydrogen (1 bar) at room temperature for 12 hr. The mixture was filtered and the filtrate was concentrated to give crude product, which was purified by pre-HPLC to give 9-(4-methyl-1H-imidazol-2-yl)-8-phenyl-8,9-dihydro-2H-pyrido[4,3,2-de]phthalazin-3(7H)-one (27 mg, yield 87%). 1H-NMR (400 MHz, CD3OD) δ (ppm): 2.22 (dd, 3H), 4.77-4.86 (m, 2H), 7.06 (s, 1H), 7.20 (d, 1H), 7.36 (t, 5H), 7.55 (d, 1H), 7.62 (t, 1H); LC-MS (ESI) m/z: 344(M+1)+.

후처리

  1. customwas purged with hydrogen (1 bar) at room temperature for 12 hr
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate was concentrated
  4. customto give crude product, which
  5. customwas purified by pre-HPLC

출처 및 근거

ORD 기록
ord-8f3e06205d5f458b89fb2107b99aa886
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012976B2

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