1-(6-Benzyloxynaphthalen-2-yl)-1-(1-trityl-1H-imidazol-4-yl)-2-methyl-1-propanol → HCID 178450081、化合物

HRID 1368524ノート

反応式

HRID 1368524 の反応式
C([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[CH:15]=[C:14]([C:19]([C:24]1[N:25]=[CH:26][N:27](C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH:28]=1)([OH:23])[CH:20]([CH3:22])[CH3:21])[CH:13]=[CH:12]2)C1C=CC=CC=1>C(O)(=O)C.[C].[Pd]>[OH:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[CH:15]=[C:14]([C:19]([C:24]1[N:25]=[CH:26][NH:27][CH:28]=1)([OH:23])[CH:20]([CH3:22])[CH3:21])[CH:13]=[CH:12]2

参加物

4

反応物 1

HCID 220183201-(6-Benzyloxynaphthalen-2-yl)-1-(1-trityl-1H-imidazol-4-yl)-2-methyl-1-propanol

生成物 1

HCID 178450081HCID 178450081、化合物収率 72.6%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 176Acetic Acid溶媒

反応条件

温度
50 °C

実験手順

1-(6-Benzyloxynaphthalen-2-yl)-1-(1-trityl-1H-imidazol-4-yl)-2-methyl-1-propanol (0.9 g) was dissolved in acetic acid (20 ml), and to the solution was added 10% palladium carbon (0.25 g). The mixture was stirred at 50° C. for 2 h under hydrogen atmosphere. The catalyst was filtered off, and the filtrate was concentrated. The residue was purified by silica gel chromatography (eluent; dichloromethane-methanol=10:1). Crystallization from methanol-ethyl acetate-diisopropyl ether gave the titled compound (0.30 g) as a colorless powder.

後処理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by silica gel chromatography (eluent; dichloromethane-methanol=10:1)
  4. customCrystallization from methanol-ethyl acetate-diisopropyl ether

出典と根拠

ORDレコード
ord-a72bfabef38f40edb4e6ae414eed708e
出典データセット
uspto-grants-2003_06
特許番号
US06573289B1

反応ノート

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