Einecs 211-027-4 → HCID 178450069、化合物

HRID 480485ノート

反応式

HRID 480485 の反応式
[CH:1]1([NH:4][C:5]([C:7]2[CH:16]=[CH:15][C:14]3[C:9](=[CH:10][CH:11]=[C:12]([C:17]([OH:45])([C:21]4[N:22]=[CH:23][N:24](C(C5C=CC=CC=5)(C5C=CC=CC=5)C5C=CC=CC=5)[CH:25]=4)[CH:18]([CH3:20])[CH3:19])[CH:13]=3)[CH:8]=2)=[O:6])[CH2:3][CH2:2]1.[Cl-].[NH+]1C=CC=CC=1.C(=O)(O)[O-].[Na+]>CO>[CH:1]1([NH:4][C:5]([C:7]2[CH:16]=[CH:15][C:14]3[C:9](=[CH:10][CH:11]=[C:12]([C:17]([OH:45])([C:21]4[N:22]=[CH:23][NH:24][CH:25]=4)[CH:18]([CH3:20])[CH3:19])[CH:13]=3)[CH:8]=2)=[O:6])[CH2:2][CH2:3]1

参加物

5

反応物 3

HCID 69401Einecs 211-027-4HCID 516892Sodium BicarbonateHCID 18769022N-cyclopropyl-6-[1-hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl)-2-naphthamide

生成物 1

HCID 178450069HCID 178450069、化合物収率 94.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

A mixture of N-cyclopropyl-6-[1-hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl)-2-naphthamide (16.0 g) and pyridinium chloride (6.46 g) in methanol (84 mL) was heated at 60° C. for 3 h. The mixture was neutralized with sodium bicarbonate solution. The solvent was evaporated and the residue was dissolved in ethanol and insoluble material was filtered off. The filtrate was concentrated and purified by column chromatography (eluent; CHCl3: 8% methanolic ammonia=19:1→9:1) to give the titled compound (8.9 g) as a colorless powder.

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe residue was dissolved in ethanol
  3. filtrationinsoluble material was filtered off
  4. concentrationThe filtrate was concentrated
  5. custompurified by column chromatography (eluent; CHCl3: 8% methanolic ammonia=19:1→9:1)

出典と根拠

ORDレコード
ord-314b47e8205c4fd99e0b721052acf9d6
出典データセット
uspto-grants-2003_11
特許番号
US06649643B1

反応ノート

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