Dichloromethane → 2-Ethoxy-4,5-dihydro-5,5-dimethyl-2-oxo-1,3,2-benzodioxaphosphepin-7-yl methanesulphonate

HRID 27638

반응식

HRID 27638 반응식
[CH3:1][S:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([C:13]([CH3:17])([CH3:16])[CH2:14][OH:15])[CH:7]=1)(=[O:4])=[O:3].C(N(CC)CC)C.[P:25](Cl)(Cl)(=[O:29])[O:26][CH2:27][CH3:28].ClCCl>C(#N)C>[CH3:1][S:2]([O:5][C:6]1[CH:11]=[CH:10][C:9]2[O:12][P:25]([O:26][CH2:27][CH3:28])(=[O:29])[O:15][CH2:14][C:13]([CH3:17])([CH3:16])[C:8]=2[CH:7]=1)(=[O:4])=[O:3]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 15158Ethyl dichlorophosphateHCID 233412804-Hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl methanesulphonate

생성물 1

HCID 233412692-Ethoxy-4,5-dihydro-5,5-dimethyl-2-oxo-1,3,2-benzodioxaphosphepin-7-yl methanesulphonate수율 44.6%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

4-Hydroxy-3-(2-hydroxy-1,1-dimethylethyl)phenyl methanesulphonate (10 g) from Example 1 was suspended in acetonitrile (100 ml) and triethylamine (8 g) was added. The mixture was cooled in ice, and ethyl phosphorodichloridate (6.9 g) was added dropwise with vigorous stirring. Stirring was continued for 6 hours prior to the addition of dichloromethane (200 ml), after which the solution was washed with water, dilute sodium hydroxide solution and water again, dried over magnesium sulphate and run down. The crude product was recrystallised from toluene, yielding 6.0 g of the desired product, melting point 113°-115° C.

후처리

  1. temperatureThe mixture was cooled in ice
  2. washafter which the solution was washed with water, dilute sodium hydroxide solution and water again
  3. dry with materialdried over magnesium sulphate
  4. customThe crude product was recrystallised from toluene

출처 및 근거

ORD 기록
ord-93e18560efd1442aa89ec305c02c79da
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04222767

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