Dimethyl Sulfate → HCID 2825022、化合物

HRID 1607629ノート

反応式

HRID 1607629 の反応式
[OH-].[Na+].S(OC)(O[CH3:7])(=O)=O.[OH:10][C:11]1[C:20]([CH3:21])=[C:19]2[C:14]([C:15](=[O:24])[CH2:16][C:17]([CH3:23])([CH3:22])[O:18]2)=[CH:13][CH:12]=1>O>[CH3:7][O:10][C:11]1[C:20]([CH3:21])=[C:19]2[C:14]([C:15](=[O:24])[CH2:16][C:17]([CH3:22])([CH3:23])[O:18]2)=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 27279747-Hydroxy-2,2,8-trimethyl-2,3-dihydro-4H-1-benzopyran-4-one

生成物 1

HCID 2825022HCID 2825022、化合物収率 78%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The reaction is carried out under nitrogen. In 50 ml of a 10% sodium hydroxide solution 4.9 g (20 millimoles) of 7-hydroxy-2,2,8-trimethyl-4-chromanone are dissolved, 2.6 g (2 ml, 21 millimoles) of dimethyl sulfate are added and the reaction mixture is vigorously stirred for 2 hours. The reaction mixture is diluted with 100 ml of icecold water and extracted three times with 50 ml of carbon tetrachloride each. The organic phase is washed twice with 50 ml of water each, dried over sodium sulfate, the solvent is removed and the residue crystallized from 90% methanol. Thus 3.4 g of the desired compound are obtained, yield 78%. Mp.: 105°-107° C.

後処理

  1. extractionextracted three times with 50 ml of carbon tetrachloride each
  2. washThe organic phase is washed twice with 50 ml of water each,
  3. dry with materialdried over sodium sulfate
  4. customthe solvent is removed
  5. customthe residue crystallized from 90% methanol

出典と根拠

ORDレコード
ord-a16aa53551be4eeab7c0b4b470865be7
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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