Methyl iodide → HCID 2825021、化合物

HRID 1607628ノート

反応式

HRID 1607628 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 2825021HCID 2825021、化合物収率 85%

試薬・触媒・溶媒 1

HCID 5462222Potassium溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d1b2ae970e3647928d1873f68bec5d4d
出典データセット
uspto-grants-1989_09
特許番号
US04866089

反応ノート

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