Propionic Acid → 2-(5,6-Dimethoxy-3,3-dimethyl-1-indanylidene)-4,4-dimethyl-3-oxo-pentanonitrile

HRID 1271791노트

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HRID 1271791 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[C:8](=O)[CH2:7][C:6]2([CH3:16])[CH3:15].[C:17]([CH2:23][C:24]#[N:25])(=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19].C(O)(=O)CC.C([O-])(=O)C.[NH4+]>C1(C)C(C)=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[C:8](=[C:23]([C:17](=[O:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[C:24]#[N:25])[CH2:7][C:6]2([CH3:16])[CH3:15]

참가 물질

6

반응물 4

HCID 1032Propionic AcidHCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-HCID 138129z1-Indanone, 5,6-dimethoxy-3,3-dimethyl-HCID 517165Ammonium Acetate

생성물 1

HCID 694270512-(5,6-Dimethoxy-3,3-dimethyl-1-indanylidene)-4,4-dimethyl-3-oxo-pentanonitrile수율 50%

시약·촉매·용매 1

HCID 7237O-Xylene용매

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온도
120 °C

실험 절차

44 g (0.2 mol) of 5,6-dimethoxy-3,3-dimethyl-1-indanone, 25 g (0.2 mol) of pivaloylacetonitrile, 32 g of propionic acid and 17 g of ammonium acetate are mixed in 80 g of xylene and heated at 120° C. for 7 hours. After the system has been cooled to room temperature and the organic phase has been washed, the xylene is distilled off, and the crude product which remains is recrystallized in methanol. Yield: 50% theory; E1/1730 (λmax 373 nm).

후처리

  1. temperatureAfter the system has been cooled to room temperature
  2. washthe organic phase has been washed
  3. distillationthe xylene is distilled off
  4. customthe crude product which remains is recrystallized in methanol

출처 및 근거

ORD 기록
ord-eb3f1430fc584b66bb8f417be2d4e2de
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07208142B2

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