N,N'-bis-(2-amino-ethyl)-N,N'-dimethyl-propane-1,3-diamine → 6-[2-({3-[(2-Amino-ethyl)-methyl-amino]-propyl}-methyl-amino)-ethylamino]-5,9-diaza-benzo[c]fluoren-7-one

HRID 496747

반응식

HRID 496747 반응식
[O:1]=[C:2]1[C:14]2[C:13](OS(C3C=CC(C)=CC=3)(=O)=O)=[N:12][C:11]3[CH:26]=[CH:27][CH:28]=[CH:29][C:10]=3[C:9]=2[C:8]2[CH:7]=[CH:6][N:5]=[CH:4][C:3]1=2.[NH2:30][CH2:31][CH2:32][N:33]([CH3:42])[CH2:34][CH2:35][CH2:36][N:37]([CH2:39][CH2:40][NH2:41])[CH3:38]>ClCCl>[NH2:41][CH2:40][CH2:39][N:37]([CH3:38])[CH2:36][CH2:35][CH2:34][N:33]([CH3:42])[CH2:32][CH2:31][NH:30][C:13]1[C:14]2[C:2](=[O:1])[C:3]3[CH:4]=[N:5][CH:6]=[CH:7][C:8]=3[C:9]=2[C:10]2[CH:29]=[CH:28][CH:27]=[CH:26][C:11]=2[N:12]=1

참가 물질

4

반응물 2

HCID 10607670N,N'-bis-(2-amino-ethyl)-N,N'-dimethyl-propane-1,3-diamineHCID 20829786toluene-4-sulfonic acid 7-oxo-7H-5,9-diaza-benzo[c]fluoren-6-yl ester

생성물 1

HCID 223220946-[2-({3-[(2-Amino-ethyl)-methyl-amino]-propyl}-methyl-amino)-ethylamino]-5,9-diaza-benzo[c]fluoren-7-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
50 °C

실험 절차

A mixture of toluene-4-sulfonic acid 7-oxo-7H-5,9-diaza-benzo[c]fluoren-6-yl ester (102 mg) (the compound of Reference Example 6c-2) and N,N′-bis-(2-amino-ethyl)-N,N′-dimethyl-propane-1,3-diamine (0.8 ml) was stirred at 50° C. for 20 minutes. The reaction mixture was diluted with dichloromethane. The solution was washed with saturated NaHCO3 solution and dried over magnesium sulfate. The organic layer was evaporated to dryness. The residue was purified by silica gel column chromatography developed by dichloromethane-methanol-ammonia water (25%)=90:10:1. The desired product (37 mg) was obtained as a reddish oil.

후처리

  1. washThe solution was washed with saturated NaHCO3 solution
  2. dry with materialdried over magnesium sulfate
  3. customThe organic layer was evaporated to dryness
  4. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-159a4154ac624503b3af81291ec50d79
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06946472B2

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