Ammonia → 2,4-Dimethylbenzene-1,3-diamine

HRID 66704

반응식

HRID 66704 반응식
C(#N)C1C=CC=C(C#[N:6])C=1.[NH3:11].[H][H].[C:14]1([CH3:21])[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[CH:15]=1>[CH-]=O.[CH-]=O.[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[C-]#[O+].[Co].[Co+2]>[C:14]1([CH3:21])[C:15]([NH2:6])=[C:16]([CH3:20])[C:17]([NH2:11])=[CH:18][CH:19]=1

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 7929M-Xylene3회HCID 12276IsophthalonitrileHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 46255812,4-Dimethylbenzene-1,3-diamine

시약·촉매·용매 1

HCID 25049Dicobalt Octacarbonyl (stabilized with 1-5% Hexane)용매

실험 절차

0.76 g of dicobalt octacarbonyl, 0.3 g of various aromatic nitriles and 20 ml of m-xylene as a solvent were charged into a 100 ml eggplant type flask equipped with a reflux condenser and a gas inlet tube, and the air was thoroughly replaced while introducing nitrogen through the gas inlet tube. Thereafter, the flask was heated in an oil bath and the temperature of oil bath was elevated to 160° C. The flask was heated for 90 minutes under reflux conditions while passing nitrogen therethrough, and then the heating was discontinued and the flask was cooled to room temperature. The precipitate formed was directly transferred into a shaking type autoclave having a net capacity of 100 ml together with solvent m-xylene. After adding 10 g of isophthalonitrile and 10 ml of m-xylene thereto, the gas in the autoclave was replaced with nitrogen. After adding 10 ml of liquid ammonia thereto, hydrogen was fed up to a pressure of 260 kg/cm2 gage and the hydrogenation of isophthalonitrile was carried out at a reaction temperature of 100° C. until no absorption of hydrogen took place. The m-xylenediamine thus formed was analyzed by gas chromatography, the results as shown in Table 1 were obtained.

후처리

  1. customequipped with a reflux condenser and a gas inlet tube
  2. additionwhile introducing nitrogen through the gas inlet tube
  3. temperatureThereafter, the flask was heated in an oil bath
  4. customthe temperature of oil bath was elevated to 160° C
  5. temperatureThe flask was heated for 90 minutes under reflux conditions
  6. customThe precipitate formed
  7. customthe hydrogenation of isophthalonitrile was carried out at a reaction temperature of 100° C. until no absorption of hydrogen

출처 및 근거

ORD 기록
ord-0236d8a247a7484099a69d9a281faa74
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343722

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