Methyl iodide → HCID 53760314、化合物

HRID 1155591

反応式

HRID 1155591 の反応式
[Mg].I[CH3:3].[C:4]1(=[O:19])[CH:18]=[CH:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH:6]=[CH:5]1.[Cl-].[NH4+]>CCOCC>[CH3:3][CH:17]1[CH2:18][C:4](=[O:19])[CH:5]=[CH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 53676690Cyclopentadeca-2,14-dien-1-one

生成物 1

HCID 53760314HCID 53760314、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

To the Grignard reagent prepared from 72 mg (3 mg-atoms) of magnesium and 0.25 ml (4 mMole) of iodomethane in 5 ml of ether was added 50 mg of cuprous iodide, and the mixture was heated at reflux for 5 min. Cyclopentadeca-2,14-dien-1-one (0.44 g; 2 mMole) in 5 ml of ether was then added over a period of 10 min without cooling, and stirring was continued for 30 min at room temperature. The reaction mixture was poured into cold ammonium chloride solution and extracted with ether. The organic layer was washed with water, dried over sodium sulphate, evaporated and distilled to give 0.33 g (69%) of dehydromuscone having b.p. 110°/0.1 Torr;

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 5 min
  3. temperaturewithout cooling
  4. extractionextracted with ether
  5. washThe organic layer was washed with water
  6. dry with materialdried over sodium sulphate
  7. customevaporated
  8. distillationdistilled
  9. customto give 0.33 g (69%) of dehydromuscone

出典と根拠

ORDレコード
ord-af6a5f61b9194d8ba3a492ec0ce7592e
出典データセット
uspto-grants-1981_11
特許番号
US04302607

関連ノート

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