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

HRID 1271791ノート

反応式

HRID 1271791 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
120 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-eb3f1430fc584b66bb8f417be2d4e2de
出典データセット
uspto-grants-2007_04
特許番号
US07208142B2

反応ノート

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