O-Xylene → RU78783

HRID 1380015

반응식

HRID 1380015 반응식
[Na].[C:2]1([CH3:9])[C:3](C)=[CH:4][CH:5]=[CH:6][CH:7]=1.[P:10]([O-:17])([O:14]CC)[O:11]CC.C(Cl)(Cl)C1C=CC=CC=1>O1CCCC1>[C:2]1([CH:9]([P:10]([OH:17])(=[O:11])[OH:14])[P:10]([OH:17])(=[O:14])[OH:11])[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 7237O-XyleneHCID 7411Benzal chlorideHCID 3780918DiethylphosphiteHCID 5360545Sodium2회

생성물 1

HCID 447537RU78783

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
62 °C

실험 절차

There were charged into the reaction vessel 23.0 grams (1.0 mole) of sodium metal along with 90 cc. of xylene and 80 cc. of tetrahydrofurane. The vessel was placed under a nitrogen blanket and 138.10 grams (1.0 mole) of diethyl phosphite added over a 35 minute period. An exothermic reaction ensued which was maintained at 62° C. by external cooling. After addition was complete the mixture was heated to 100° C. and held there until all of the sodium metal was gone. The mixture was cooled to 60° to 70° C. and 80.50 grams (0.5 ,ole) of benzal chloride were added gradually over a 25 minute period. An exothermic reaction ensued which was maintained at 60° to 70° C. by external cooling. The mixture was then heated for 4 hours at 70° to 75° C., cooled to 60° C. The liquid material was separated from the solid and the solid boiled 8 times with 100 cc. of benzene to extract the organic material. The eluate product was then distilled, terminal conditions being a pot temperature of 201° C., distillate temperature 125° C. and pressure 6 mm. The solid residue of 70 grams was tetraethyl phenyl methane diphosphonate. This product was hydrolyzed and the hydrolysis product purifid as in Example 1 to obtain phenyl methane diphosphonic acid.

후처리

  1. additionadded over a 35 minute period
  2. customAn exothermic reaction
  3. additionAfter addition
  4. temperaturewas heated to 100° C.
  5. temperatureThe mixture was cooled to 60° to 70° C.
  6. customAn exothermic reaction
  7. temperaturewas maintained at 60° to 70° C. by external cooling
  8. temperatureThe mixture was then heated for 4 hours at 70° to 75° C.
  9. temperaturecooled to 60° C
  10. customThe liquid material was separated from the solid
  11. extractionof benzene to extract the organic material
  12. distillationThe eluate product was then distilled
  13. customa pot temperature of 201° C., distillate temperature 125° C. and pressure 6 mm

출처 및 근거

ORD 기록
ord-d394fb67cabd4032aa1d696a59a6b9ab
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579720

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