Dimethylamine → (Dihydro-3,3-diphenyl-3H-furan-2-ylidene)dimethylammonium bromide

HRID 279074

반응식

HRID 279074 반응식
[CH3:1][NH:2][CH3:3].C(=O)([O-])[O-].[Na+].[Na+].[Br:10][CH2:11][CH2:12][C:13]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:14](Cl)=[O:15]>O.C1(C)C=CC=CC=1>[Br-:10].[CH3:1][N+:2]([CH3:3])=[C:14]1[C:13]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:12][CH2:11][O:15]1

참가 물질

6

반응물 3

HCID 674DimethylamineHCID 10340Sodium CarbonateHCID 222500664-Bromo-2,2-diphenylbutyric chloride2회

생성물 1

HCID 2723589(Dihydro-3,3-diphenyl-3H-furan-2-ylidene)dimethylammonium bromide수율 46.8%

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

반응 조건

온도
2.5 °C

실험 절차

In 100 mL of water were suspended 8 g (90 mmol) of a 50% aqueous solution of dimethylamine and 18 g (170 mmol) of sodium carbonate, followed by cooling to 0 to 5° C. A solution obtained by dissolving 23 g (68 mmol) of the 4-bromo-2,2-diphenylbutyric chloride mentioned above in 100 mL of toluene was then added dropwise. After stirring for 2 hours, the water layer taken out from the reaction mixture was washed with toluene. The resulting water layer was extracted with chloroform. The extract was washed with water and then dried. The residue obtained by concentrating the solvent under reduced pressure was crystallized from methyl isobutyl ketone, whereby 11 g (yield: 46.8%) of dimethyl(tetrahydro-3,3-diphenyl-2-furylidene)ammonium bromide was obtained.

후처리

  1. customA solution obtained
  2. additionwas then added dropwise
  3. washwas washed with toluene
  4. extractionThe resulting water layer was extracted with chloroform
  5. washThe extract was washed with water
  6. customdried
  7. customThe residue obtained
  8. concentrationby concentrating the solvent under reduced pressure
  9. customwas crystallized from methyl isobutyl ketone

출처 및 근거

ORD 기록
ord-59e7d6bdf1514172bcd3af8ded68a246
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06362203B1

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