Methyl iodide → HCID 53760314, 화합물

HRID 1155591노트

반응식

HRID 1155591 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 53760314HCID 53760314, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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;

후처리

  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

출처 및 근거

ORD 기록
ord-af6a5f61b9194d8ba3a492ec0ce7592e
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04302607

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