홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Glyoxal → HCID 19101917, 화합물

HRID 1974663
노트
인쇄 미리보기

반응식

HRID 1974663 반응식
N[C:2]1[C:11]([NH2:12])=[CH:10][CH:9]=[C:4]([C:5]([O:7][CH3:8])=[O:6])[C:3]=1[C:13]([O:15][CH3:16])=[O:14].C(C=O)=O.O1C[CH2:24][CH2:23][CH2:22]1>O>[N:12]1[C:11]2[C:2](=[C:3]([C:13]([O:15][CH3:16])=[O:14])[C:4]([C:5]([O:7][CH3:8])=[O:6])=[CH:9][CH:10]=2)[CH:24]=[CH:23][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7860GlyoxalHCID 8028TetrahydrofuranHCID 145744761,2-Benzenedicarboxylic acid, 3,4-diamino-, 1,2-dimethyl ester

생성물 1

HCID 19101917HCID 19101917, 화합물수율 78.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of dimethyl 3,4-diaminophthalate (11.2 g, 0.05 mol) in tetrahydrofuran is treated with glyoxal (2.9 g, 0.05 mol) in water at reflux temperature, stirred for 4 hours at reflux temperature and overnight at room temperature, and concentrated in vacuo. The resultant residue is partitioned between water and methylene chloride. The organic phase is dried (MgSO4) and concentrated in vacuo to give a brown solid residue. Recrystallization from methanol gives the title product as a pink powder (9.67 g, 78.6%) mp 124°-125° C., identified by H1NMR, C13NMR, and IR spectral analyses.

후처리

  1. temperatureat reflux temperature
  2. concentrationconcentrated in vacuo
  3. customThe resultant residue is partitioned between water and methylene chloride
  4. dry with materialThe organic phase is dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customto give a brown solid residue
  7. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-c952ba58284f4fbabd0a85edd5a32a67
출처 데이터셋
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05283335

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트