Hydrochloric Acid → HCID 13627533, 화합물

HRID 1589617노트

반응식

HRID 1589617 반응식
[C:1]([C:3]1[C:8]([F:9])=[C:7]([F:10])[C:6]([OH:11])=[C:5]([F:12])[C:4]=1[F:13])#[N:2].[C:14](Cl)(=[O:18])[C:15]([CH3:17])=[CH2:16].C(=O)([O-])[O-].[Ca+2].Cl>C1C=CC=CC=1>[C:14]([O:11][C:6]1[C:5]([F:12])=[C:4]([F:13])[C:3]([C:1]#[N:2])=[C:8]([F:9])[C:7]=1[F:10])(=[O:18])[C:15]([CH3:17])=[CH2:16]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 10112Calcium CarbonateHCID 13528Methacryloyl chlorideHCID 3613333Benzonitrile, 2,3,5,6-tetrafluoro-4-hydroxy-

생성물 1

HCID 13627533HCID 13627533, 화합물수율 63.9%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

In 30 ml of benzene, 3.0 g (0.0157 mol) of 4-cyano-2,3,5,6-tetrafluorophenol and 1.80 g (0.0173 mol) of methacrylic acid chloride were dissolved. The resultant solution, and 1.73 g (0.0173 mol) of calcium carbonate added thereto as a hydrogen chloride trapping agent were stirred under reflux for 32 hours. The resultant reaction mixture was cooled off and filtered to separate calcium carbonate. The filtrate was dried with magnesium sulfate and then evaporated with a rotary evaporator. Consequently, there was obtained 2.6 g of 4-cyano-2,3,5,6-tetrafluorophenyl methacrylate (yeild 63.9% and purity 95.4%). The analyses obtained of the novel substance for the determination of its chemical structure were the same as those of Example 2.

후처리

  1. temperatureunder reflux for 32 hours
  2. customThe resultant reaction mixture
  3. temperaturewas cooled off
  4. filtrationfiltered
  5. customto separate calcium carbonate
  6. dry with materialThe filtrate was dried with magnesium sulfate
  7. customevaporated with a rotary evaporator

출처 및 근거

ORD 기록
ord-bb95f3264134436e971880920d32f9bb
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04572805

반응 노트

불러오는 중…