Methyl iodide → HCID 2825021, 화합물

HRID 1073374노트

반응식

HRID 1073374 반응식
[C:1](#N)C.C1OCCOCCOCCOCCOCCOC1.CI.[OH:24][C:25]1[CH:34]=[C:33]2[C:28]([C:29](=[O:37])[CH2:30][C:31]([CH3:36])([CH3:35])[O:32]2)=[C:27]([CH3:38])[CH:26]=1>[K]>[CH3:1][O:24][C:25]1[CH:34]=[C:33]2[C:28]([C:29](=[O:37])[CH2:30][C:31]([CH3:35])([CH3:36])[O:32]2)=[C:27]([CH3:38])[CH:26]=1

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 6342AcetonitrileHCID 2855718-Crown-6HCID 27279647-Hydroxy-2,2,5-trimethyl-2,3-dihydro-4H-1-benzopyran-4-one

생성물 1

HCID 2825021HCID 2825021, 화합물수율 85%

시약·촉매·용매 1

HCID 5462222Potassium용매

실험 절차

In 50 ml of acetonitrile 4.9 g (20 millimoles) of the potassium salt of 7-hydroxy-2,2,5-trimethyl-4-chromanone are dissolved and the solution is stirred in the presence of 0.5 g (2 millimoles) of 18-Crown-6 at room temperature for 30 minutes. To the mixture 4.25 g (1.9 ml, 30 millimoles) of methyl iodide are added and the reaction mixture is stirred for a further hour. The inorganic salt is filtered off and the solvent is removed. The residue is taken up in chloroform, washed twice with 50 ml of water each, dried over sodium sulfate and evaporated. The product is crystallized from 90% ethanol. Thus 3.75 g of the desired compound are obtained, yield 85%. Mp.: 86°-88° C.

후처리

  1. filtrationThe inorganic salt is filtered off
  2. customthe solvent is removed
  3. washwashed twice with 50 ml of water each,
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customThe product is crystallized from 90% ethanol

출처 및 근거

ORD 기록
ord-35fe67c2516f4b09a9166ebff765d40a
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04968819

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