Hydrogen Bromide → HCID 20145262, 화합물

HRID 648638노트

반응식

HRID 648638 반응식
N([O-])=O.[Na+].N[C:6]1[CH:7]=[CH:8][C:9]([N:27]2[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]2)=[C:10]([CH:12]([CH:14]([C:24]([NH2:26])=[O:25])[C:15]2[CH:23]=[CH:22][C:18]([C:19]([OH:21])=[O:20])=[CH:17][CH:16]=2)[CH3:13])[CH:11]=1.[OH-].[Na+].[BrH:35]>O.[Cu]Br>[Br:35][C:6]1[CH:7]=[CH:8][C:9]([N:27]2[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]2)=[C:10]([CH:12]([CH:14]([C:24]([NH2:26])=[O:25])[C:15]2[CH:23]=[CH:22][C:18]([C:19]([OH:21])=[O:20])=[CH:17][CH:16]=2)[CH3:13])[CH:11]=1

참가 물질

7

반응물 4

HCID 260Hydrogen Bromide2회HCID 14798Sodium HydroxideHCID 20145241HCID 20145241, 화합물HCID 23668193Sodium Nitrite

생성물 1

HCID 20145262HCID 20145262, 화합물

시약·촉매·용매 2

HCID 24593copper(I) bromide촉매HCID 962Water용매

실험 절차

A solution of 0.072 gm (1.05 m mol) of sodium nitrite in 0.5 ml of water was added dropwise at an internal temperature of 0° to 5° C. to 0.40 gm (1.05 m mol) of 4-[(1-(5-amino-2-piperidino-phenyl)-ethyl)-aminocarbonylmethyl]-benzoic acid in 2 ml of semi-concentrated aqueous hydrobromic acid. The thus obtained diazonium salt solution was then added dropwise to 0.196 gm of copper-(I) bromide in 2 ml of 48% hydrobromic acid, whereby strong formation of gas occurred. The reaction mixture was stirred for 1.5 hours at an internal temperature of 45° to 50° C., cooled, and adjusted to pH 4 by means of 4N sodium hydroxide solution. After extraction with warm ethyl acetate, the extract was washed with water, dried, and filtered. After evaporation in vacuo, the residue obtained was purified by column chromatography on silica gel (chloroform/methanol=7:1).

후처리

  1. temperaturecooled
  2. extractionAfter extraction with warm ethyl acetate
  3. washthe extract was washed with water
  4. customdried
  5. filtrationfiltered
  6. customAfter evaporation in vacuo
  7. customthe residue obtained
  8. customwas purified by column chromatography on silica gel (chloroform/methanol=7:1)

출처 및 근거

ORD 기록
ord-35d78875dcd5464793779c4b5b06333b
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735959

반응 노트

불러오는 중…