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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dimethylformamide → HCID 131718228, 화합물

HRID 1656446
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HRID 1656446 반응식
Cl.Cl.[NH2:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([NH2:9])=N.C[N:14](C=O)C.[C:18]1(=[O:25])[O:24][C:22](=[O:23])[CH2:21][CH2:20][CH2:19]1>CN(C1C=CC=CN=1)C.N1C=CC=CC=1>[NH2:14][N:9]=[CH:7][C:6]1[CH:5]=[C:4]([NH:3][CH:21]([CH:22]=[O:23])[CH2:20][CH2:19][C:18]([OH:24])=[O:25])[CH:12]=[CH:11][CH:10]=1
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참가 물질

6

반응물 3

HCID 6228DimethylformamideHCID 7940Glutaric anhydrideHCID 3084651m-Aminobenzamidine dihydrochloride

생성물 1

HCID 131718228HCID 131718228, 화합물수율 90%

시약·촉매·용매 2

HCID 218852-Dimethylaminopyridine촉매HCID 1049Pyridine용매

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온도
100 °C

실험 절차

3-Aminobenzamidine di-HCL (5 g, 24 mmol) was added to dry DMF (30 mL). To this solution dry pyridine (5 mL) and glutaric anhydride (3.0 g, 26 mmol), followed by 10 mg dimethylaminopyridine (DMAP) were added. The product was heated for 3 h at 100° C. and allowed to stir at room temperature for 16 h. Solvents were removed in vacuo, water was added to the residue and the pH was brought to a value of 6.8 using dilute sodium hydroxide. An abundant precipitate was filtered, washed with water followed by ethyl acetate. The white solid was filtered and dried in a desiccator to give 5.4 g, 90% of product as a white solid: 1H NMR (d6 -DMSO) δ 1.8 (m, 2H), 2.3 (m, 2H), 2.45 (m, 2H), 7.6 (d, 1H, J=8 Hz), 7.55 (dd, 1H, J=8 Hz and J= 7.5 Hz), 7.85 (d, 1H, J=7.5 Hz), 8.05 (s, 1H), 9.05 (bs, 2H), 9.25 (bs, 2H), 10.4 (s, 1H); MS (FAB) m/e 250.1 (MH+).

후처리

  1. additionwere added
  2. customSolvents were removed in vacuo, water
  3. additionwas added to the residue
  4. filtrationAn abundant precipitate was filtered
  5. washwashed with water
  6. filtrationThe white solid was filtered
  7. customdried in a desiccator

출처 및 근거

ORD 기록
ord-7ee2fe3b36b54da783dc9ea5a6ff82c6
출처 데이터셋
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05254573

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