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Tetrahydrofuran → N,N'-didecyl-5-nitro-1,3-benzenedicarboxamide

HRID 1110218
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HRID 1110218 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:13]([OH:15])=O)[CH:7]=[C:8]([CH:12]=1)[C:9]([OH:11])=O)([O-:3])=[O:2].[CH2:16]([NH2:26])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].C([N:29]([CH2:32][CH3:33])CC)C.O1[CH2:38][CH2:37][CH2:36][CH2:35]1>S(Cl)(Cl)=O.O.CN(C=O)C>[CH2:16]([NH:26][C:9]([C:8]1[CH:12]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=[C:6]([C:13]([NH:29][CH2:32][CH2:33][CH2:35][CH2:36][CH2:37][CH2:38][CH2:5][CH2:4][CH2:12][CH3:8])=[O:15])[CH:7]=1)=[O:11])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 8916DecylamineHCID 120695-Nitroisophthalic acid

생성물 1

HCID 19388993N,N'-didecyl-5-nitro-1,3-benzenedicarboxamide수율 150.2%

시약·촉매·용매 3

HCID 962Water용매
HCID 6228
Dimethylformamide
용매
HCID 24386Thionyl Chloride용매

실험 절차

To 30 g (0.14 mol) of 5-nitroisophthalic acid suspended in 120 ml of thionyl chloride was added 2 ml of DMF and the solution was stirred at reflux for 3.5 hours. The excess thionyl chloride was removed at reduced pressure and the residue acid chloride was dissolved in 220 ml of anhydrous tetrahydrofuran. This solution was added dropwise to 64 ml (0.32 mol) of decyl amine and 44 ml (0.32 mol) of triethylamine in 350 mol of anhydrous tetrahydrofuran over 30 minutes with ice bath cooling. The reaction mixture was stirred at room temperature for 4 hours and then poured into 3 L of water. The resultant solid was removed by filtration and recrystallized from methanol to give 51.5 g (74% yield, mp 115°-116°) of N,N'-didecyl-5-nitro-1,3-benzenedicarboxamide.

후처리

  1. temperatureat reflux for 3.5 hours
  2. customThe excess thionyl chloride was removed at reduced pressure
  3. dissolutionthe residue acid chloride was dissolved in 220 ml of anhydrous tetrahydrofuran
  4. temperaturecooling
  5. stirringThe reaction mixture was stirred at room temperature for 4 hours
  6. customThe resultant solid was removed by filtration
  7. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-877bba8994ec41448896d18659791015
출처 데이터셋
uspto-grants-1994_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05324747

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