Pentanenitrile, 4,4-dimethyl-3-oxo- → HCID 66644209、化合物

HRID 883021ノート

反応式

HRID 883021 の反応式
[ClH:1].Cl.[CH:3]1([CH2:6][NH:7][NH2:8])[CH2:5][CH2:4]1.[CH3:9][C:10]([CH3:17])([CH3:16])[C:11](=O)[CH2:12][C:13]#[N:14]>C(O)C>[ClH:1].[C:10]([C:11]1[CH:12]=[C:13]([NH2:14])[N:7]([CH2:6][CH:3]2[CH2:5][CH2:4]2)[N:8]=1)([CH3:17])([CH3:16])[CH3:9]

参加物

4

反応物 2

HCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-HCID 43810474(Cyclopropylmethyl)hydrazine--hydrogen chloride (1/2)

生成物 1

HCID 66644209HCID 66644209、化合物収率 90%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of Example 1B (13.5 g, 85 mmol) and 4,4-dimethyl-3-oxopentanenitrile (11.7 g, 93 mmol) in ethanol (100 mL) was heated at reflux for 6 hours. The mixture was cooled to room temperature, and concentrated under reduced pressure. The residue was diluted with ethyl acetate (20 mL). The resulting white precipitate was filtered, washed with ether, and dried to yield 17.5 g (90%) of title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 0.42-0.54 (m, 4 H), 1.16-1.27 (m, 1 H), 1.28 (s, 9 H), 4.38 (d, J=7.12 Hz, 2 H), 4.80 (br, 2 H), 5.53 (s, 1 H), 15.5 (br, 1 H); MS (DCI) m/z 194 [M+H]+.

後処理

  1. temperatureat reflux for 6 hours
  2. concentrationconcentrated under reduced pressure
  3. additionThe residue was diluted with ethyl acetate (20 mL)
  4. filtrationThe resulting white precipitate was filtered
  5. washwashed with ether
  6. customdried

出典と根拠

ORDレコード
ord-f4f76006a7f142d0a4fc517c89a5c429
出典データセット
uspto-grants-2012_08
特許番号
US08236822B2

反応ノート

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