Hydrochloric Acid → HCID 19033222, 화합물

HRID 266605

반응식

HRID 266605 반응식
[CH:1]1[C:18]2=[C:19]3[C:8]([C:9]4[C:20]5[C:13](=[CH:14][CH:15]=[CH:16][C:17]2=5)[CH:12]=[CH:11][CH:10]=4)=[CH:7][CH:6]=[C:5]2[C:21]([O:23][C:24](=O)[C:3](=[C:4]23)[CH:2]=1)=[O:22].[C:26]([C:30]1[CH:36]=[CH:35][C:33]([NH2:34])=[CH:32][CH:31]=1)([CH3:29])([CH3:28])[CH3:27].N1C=CN=C1.Cl>O.O.C([O-])(=O)C.[Zn+2].C([O-])(=O)C.C(O)C>[C:26]([C:30]1[CH:31]=[CH:32][C:33]([N:34]2[C:21](=[O:22])[C:5]3[C:4]4[C:19]5[C:8](=[CH:7][CH:6]=3)[C:9]3[C:20]6[C:13]([CH:12]=[CH:11][CH:10]=3)=[CH:14][CH:15]=[CH:16][C:17]=6[C:18]=5[CH:1]=[CH:2][C:3]=4[C:24]2=[O:23])=[CH:35][CH:36]=1)([CH3:29])([CH3:27])[CH3:28]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 795ImidazoleHCID 698614-Tert-ButylanilineHCID 11759069Perylene-3,4-dicarboxylic anhydride

생성물 1

HCID 19033222HCID 19033222, 화합물수율 81.3%

시약·촉매·용매 2

HCID 2724192Zinc acetate (USP)촉매HCID 702Ethanol용매2회

실험 절차

0.70 g (2.17 mmol) of perylene-3,4-dicarboxylic anhydride is mixed with 0.49 g (3.28 mmol) of 4-t-butylaniline, 3.00 g of imidazole and 0.10 g of zinc acetate dihydrate and the mixture is heated at 140°-150° C. for 5 h. While still hot, the mixture is treated with 100 ml of ethanol, and then 200 ml of 10% hydrochloric acid are added. The red suspension is heated until all the ethanol has evaporated, and the product is then filtered off with suction. The red-brown residue is boiled in 10% potassium carbonate solution, the solid residue is filtered off with suction while hot and rinsed several times with hot dist. water. The red residue is dried in a drying cabinet at 120° C. and then recrystallized by extraction with a toluene/methanol mixture to give 0.80 g (81%) of red N-(4-t-butylphenyl)perylene-3,4-dicarboximide which shows a red solid fluorescence. M.p. >330° C. Rf (CHCl3 /silica gel)=0.35.

후처리

  1. temperaturethe mixture is heated at 140°-150° C. for 5 h
  2. customhas evaporated
  3. filtrationthe product is then filtered off with suction
  4. filtrationthe solid residue is filtered off with suction while hot and
  5. washrinsed several times with hot dist
  6. customThe red residue is dried in a drying cabinet at 120° C.
  7. customrecrystallized by extraction with a toluene/methanol mixture

출처 및 근거

ORD 기록
ord-16dd334854764a0590178515dbeeb052
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05650513

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