Einecs 211-027-4 → HCID 178450069, 화합물

HRID 480485노트

반응식

HRID 480485 반응식
[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

참가 물질

5

반응물 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

생성물 1

HCID 178450069HCID 178450069, 화합물수율 94.2%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-314b47e8205c4fd99e0b721052acf9d6
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06649643B1

반응 노트

불러오는 중…