Acetic Acid → (3,3-Dimethylbutan-2-ylidene)propanedinitrile

HRID 236225

반응식

HRID 236225 반응식
[C:1](#[N:5])[CH2:2][C:3]#[N:4].[CH3:6][C:7]([CH3:12])([CH3:11])[C:8](=O)[CH3:9].C([O-])(=O)C.[NH4+].C(O)(=O)C>C1(C)C=CC=CC=1>[CH3:6][C:7]([C:8]([CH3:9])=[C:2]([C:1]#[N:5])[C:3]#[N:4])([CH3:12])[CH3:11]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 6416PinacoloneHCID 8010MalononitrileHCID 517165Ammonium Acetate

생성물 1

HCID 534326(3,3-Dimethylbutan-2-ylidene)propanedinitrile수율 68.4%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A solution of 9.9 g of malononitrile, 26.25 g of 3,3-dimethyl-2-butanone, 1.45 g of ammonium acetate and 2.25 g of acetic acid dissolved in 100 ml of toluene was refluxed for about 16 hours with the aid of a Dean-Stark Trap. The reaction mixture was diluted with 120 ml of toluene and washed with 200 ml water. The organic phase was collected, dried over anhydrous magnesium sulfate, filtered and concentrated under vacuum. The resulting residue was distilled under vacuum to afford 15.2 g of 2-(1,1-dimethylethyl)-1,1-dicyano-1-propene as an oil. Yield 68%.

후처리

  1. temperaturewas refluxed for about 16 hours with the aid of a Dean-Stark Trap
  2. washwashed with 200 ml water
  3. customThe organic phase was collected
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. distillationThe resulting residue was distilled under vacuum

출처 및 근거

ORD 기록
ord-aa5428eb78a445e4ae7e7564a987dd8c
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04643758

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