Silane, bromotriethyl- → N-(2,3-Dioxo-7-nitro-1,2,3,4-tetrahydroquinoxalin-5-ylmethyl)-alpha-(ethylamino)ethylphosphonic acid hydrobromide

HRID 1953774

반응식

HRID 1953774 반응식
[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([N:8]=[C:9]([O:16]C)[C:10]([O:14]C)=[N:11]2)=[C:6]([CH2:18][N:19]([CH2:28][CH3:29])[CH:20]([P:22](=[O:27])([O:25]C)[O:23]C)[CH3:21])[CH:5]=1)([O-:3])=[O:2].C([Si](CC)(CC)[Br:33])C>ClCCl>[BrH:33].[O:14]=[C:10]1[C:9](=[O:16])[NH:8][C:7]2[C:12](=[CH:13][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]=2[CH2:18][N:19]([CH2:28][CH3:29])[CH:20]([P:22](=[O:23])([OH:25])[OH:27])[CH3:21])[NH:11]1

참가 물질

4

실험 절차

160 mg (0.37 mmol) of dimethyl N-(7-nitro-2,3-dimethoxyquinoxalin-5-ylmethyl)-α-(ethylamino)ethylphosphonate are dissolved in 8 ml of dichloromethane and stirred at room temperature for one hour with 0.19 ml (4 eq.) of triethylbromosilane. The solvent and excess reagent are evaporated and the residue is briefly dried in a high vacuum, dissolved in 5 ml of an about 33% hydrogen bromide solution in acetic acid, and stirred at room temperature for 18 hours. The reaction mixture is diluted with diethyl ether, and the solid is filtered off, washed with diethyl ether and dried. The title compound is obtained as a beige solid; m.p.=191° (dec.).

후처리

  1. customThe solvent and excess reagent are evaporated
  2. customthe residue is briefly dried in a high vacuum
  3. dissolutiondissolved in 5 ml of an about 33% hydrogen bromide solution in acetic acid
  4. additionThe reaction mixture is diluted with diethyl ether
  5. filtrationthe solid is filtered off
  6. washwashed with diethyl ether
  7. customdried

출처 및 근거

ORD 기록
ord-805450e2d57f40898fcf73124a490141
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06117873

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