Diisobutylamine → HCID 21272460, 화합물

HRID 1193538

반응식

HRID 1193538 반응식
[N+:1]([C:4]1[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-:15])=[O:14])[C:5]=1[C:6]([OH:8])=O)([O-:3])=[O:2].[CH2:16]([NH:20][CH2:21][CH:22]([CH3:24])[CH3:23])[CH:17]([CH3:19])[CH3:18].P(Cl)(Cl)(Cl)=O.C([O-])(O)=O.[Na+]>C1(C)C=CC=CC=1>[CH2:16]([N:20]([CH2:21][CH:22]([CH3:24])[CH3:23])[C:6](=[O:8])[C:5]1[C:9]([N+:13]([O-:15])=[O:14])=[CH:10][CH:11]=[CH:12][C:4]=1[N+:1]([O-:3])=[O:2])[CH:17]([CH3:19])[CH3:18]

참가 물질

6

반응물 4

HCID 8085DiisobutylamineHCID 24813Phosphorus oxychlorideHCID 119206Benzoic acid, 2,6-dinitro-HCID 516892Sodium Bicarbonate

생성물 1

HCID 21272460HCID 21272460, 화합물수율 64.8%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
50 °C

실험 절차

To a slurry of 106.5 g of 2,6-dinitrobenzoic acid in 1000 ml of toluene was added with stirring 133.2 g of diisobutylamine. Next 44.9 g of phosphorus oxychloride was added dropwise at such a rate to maintain the temperature below 40° C. The mixture was heated to 50° C. for 12 hrs and poured into 500 ml of aqueous 5% NaHCO3 solution with stirring. The organic layer was separated, washed with 500 ml water, and the toluene removed under reduced pressure. The remaining solid was recrystallized from hot ethanol to give 105.2 g of N,N-diisobutyl-2,6-dinitrobenzamide, a yellow solid, mp 97°-99° C.

후처리

  1. temperatureto maintain the temperature below 40° C
  2. customThe organic layer was separated
  3. washwashed with 500 ml water
  4. customthe toluene removed under reduced pressure
  5. customThe remaining solid was recrystallized from hot ethanol

출처 및 근거

ORD 기록
ord-2c7d3a4bb767437e821819555240276b
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04810769

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