Triethylamine → N-(7-bromo-2,3-dimethoxy-quinoxalin-5-ylmethyl)-oxalamic acid ethyl ester

HRID 1422227노트

반응식

HRID 1422227 반응식
Cl.[NH2:2][CH2:3][C:4]1[CH:13]=[C:12]([Br:14])[CH:11]=[C:10]2[C:5]=1[N:6]=[C:7]([O:17][CH3:18])[C:8]([O:15][CH3:16])=[N:9]2.C(N(CC)CC)C.[Cl-].[CH2:27]([O:29][C:30](=[O:34])[C:31](O)=[O:32])[CH3:28]>C1COCC1>[CH2:27]([O:29][C:30](=[O:34])[C:31]([NH:2][CH2:3][C:4]1[CH:13]=[C:12]([Br:14])[CH:11]=[C:10]2[C:5]=1[N:6]=[C:7]([O:17][CH3:18])[C:8]([O:15][CH3:16])=[N:9]2)=[O:32])[CH3:28]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 18706309HCID 18706309, 화합물HCID 23618337Oxalic acid monoethylester chloride

생성물 1

HCID 54297612N-(7-bromo-2,3-dimethoxy-quinoxalin-5-ylmethyl)-oxalamic acid ethyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

300 mg (1 mmol) of 5-aminomethyl-7-bromo-2,3-dimethoxyquinoxaline hydrochloride are suspended in 10 ml of THF and the suspension is cooled to 0° C. 0.183 ml (1.3 equiv.) of triethylamine is added and then 0.123 ml (1.1 equiv.) of oxalic acid monoethyl ester chloride is added dropwise in the course of 30 minutes. The mixture is stirred at 0° C. for 2 hours, then at 20° C. for 16 hours and is concentrated by evaporation. The residue is stirred in diethyl ether, and the solid is filtered off, washed with water and diethyl ether and dried.

후처리

  1. waitat 20° C. for 16 hours
  2. concentrationis concentrated by evaporation
  3. stirringThe residue is stirred in diethyl ether
  4. filtrationthe solid is filtered off
  5. washwashed with water and diethyl ether
  6. customdried

출처 및 근거

ORD 기록
ord-3a4eeae901ef4f8f8829ea663f2041ce
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06080743

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