Hydrochloric Acid → Phthalonitrile

HRID 1488899노트

반응식

HRID 1488899 반응식
O[C:2]1[CH:3]=[C:4]([C:10]#[N:11])[C:5](=[CH:8][CH:9]=1)[C:6]#[N:7].C(=O)([O-])[O-].[K+].[K+].ClCC[Si](C)(C)C.Cl>CN(C)C=O>[C:10](#[N:11])[C:4]1[C:5](=[CH:8][CH:9]=[CH:2][CH:3]=1)[C:6]#[N:7]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 38757654-Hydroxybenzene-1,2-dicarbonitrileHCID 11040763(2-Chloroethyl)trimethylsilane

생성물 1

HCID 7042Phthalonitrile수율 138.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In 200 ml of N,N-dimethylformamide were dissolved with heating 20 g of 4-hydroxyphthalonitrile and 10.55 g of potassium carbonate, to which 20 g of chloroethyl-trimethylsilane were added dropwise at 40° C. in the atmosphere of argon. Immediately after the addition, the mixture was stirred for 18 hours while maintaining the reaction temperature at 85°-105° C. The reaction vessel was then cooled to room temperature and 250 ml of dilute hydrochloric acid was added. The mixture was extracted with 1.2 liters of toluene. The organic layer was washed well with water and water was removed with magnesium sulfate. Thereafter, toluene was removed by distillation and the residue was purified with a toluene/silica gel column to obtain 24.6 g (yield: 77.0%) of a compound having the formula (XVII) below. ##STR39##

후처리

  1. additionImmediately after the addition
  2. temperaturewhile maintaining the reaction temperature at 85°-105° C
  3. extractionThe mixture was extracted with 1.2 liters of toluene
  4. washThe organic layer was washed well with water and water
  5. customwas removed with magnesium sulfate
  6. customThereafter, toluene was removed by distillation
  7. customthe residue was purified with a toluene/silica gel column

출처 및 근거

ORD 기록
ord-6710cbc9b6b34e5b884915a53eb1882f
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677025

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