Triethylamine → HCID 86747961, 화합물

HRID 1110308

반응식

HRID 1110308 반응식
[N+:1]([C:4]1[CH:12]=[C:11]([C:13]([OH:15])=O)[CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=O)([O-:3])=[O:2].S(Cl)(Cl)=O.[CH2:20]([NH2:30])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29].C([N:33]([CH2:36][CH3:37])CC)C>C1COCC1.O.CN(C=O)C>[CH2:20]([NH:30][C:6]([C:5]1[CH:9]=[CH:10][C:11]([C:13]([NH:33][CH2:36][CH2:37][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])=[O:15])=[CH:12][C:4]=1[N+:1]([O-:3])=[O:2])=[O:8])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29]

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 8916DecylamineHCID 24386Thionyl ChlorideHCID 691221,4-Benzenedicarboxylic acid, 2-nitro-

생성물 1

HCID 86747961HCID 86747961, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매2회

실험 절차

A mixture of 10 g (0.047 mol) of nitroterephthalic acid, 40 ml of thionyl chloride and 1 ml of anhydrous DMF was stirred at reflux for 5 hours. The reaction mixture was concentrated at reduced pressure and the residual acid chloride was dissolved in anhydrous THF and added dropwise over 30 minutes to a stirred, ice bath cooled solution of 25 ml (0.126 mol) of decylamine and 15 ml (0.108 mol) of triethylamine in 100 ml of anhydrous THF. Additional THF (50 ml) was added and stirring was continued for 17 hours at room temperature. Water (1 L) was added and the precipitate was filtered and recrystallized from methanol-water to give 20.4 g, mp 159°-160° of N-[2,5-bis[(decylamino)carbonyl]nitrobenzene.

후처리

  1. temperatureat reflux for 5 hours
  2. concentrationThe reaction mixture was concentrated at reduced pressure
  3. dissolutionthe residual acid chloride was dissolved in anhydrous THF
  4. additionadded dropwise over 30 minutes to a stirred, ice bath
  5. stirringstirring
  6. filtrationthe precipitate was filtered
  7. customrecrystallized from methanol-water

출처 및 근거

ORD 기록
ord-a306068801e24b96904eccee9862a2a9
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05324747

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