Dimethyl Sulfate → HCID 2825022, 화합물

HRID 1607629노트

반응식

HRID 1607629 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 2825022HCID 2825022, 화합물수율 78%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a16aa53551be4eeab7c0b4b470865be7
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04866089

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