Sodium Hydroxide → HCID 16781333, 화합물

HRID 456588

반응식

HRID 456588 반응식
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][CH:2]1C=O.[CH3:13][O:14]S([O-])(=O)=O.[CH3:19][S+](C)C.[OH-].[Na+]>ClCCl>[O:14]1[CH2:13][CH:19]1[C:8]1[CH:9]=[CH:10][C:5]2[O:4][CH2:3][CH2:2][O:1][C:6]=2[CH:7]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 1917252-Formyl-1,4-benzodioxaneHCID 2760871Trimethylsulfonium methyl sulfate

생성물 1

HCID 16781333HCID 16781333, 화합물수율 100.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 1,4-benzodioxanecarboxaldehyde [RN 29668-44-8](1.5 g, 9.14 mmol), trimethylsulfonium methyl sulfate (2.24 g, 11.9 mmol), dichloromethane (35 ml) and 50% aqueous sodium hydroxide (5 ml) were vigorously stirred for 70 hours. The mixture was partitioned between water and diethyl ether and the layers separated. The aqueous phase was extracted with diethyl ether. The combined organic phases were washed with water, brine, then dried over magnesium sulfate and evaporated to give crude 6-oxiranyl-2,3-dihydro-benzo[1,4]dioxine (1.64 g, 100%).

후처리

  1. customThe mixture was partitioned between water and diethyl ether
  2. customthe layers separated
  3. extractionThe aqueous phase was extracted with diethyl ether
  4. washThe combined organic phases were washed with water, brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

출처 및 근거

ORD 기록
ord-6c474692bdbe4f82b3b6d1648d1a2bc8
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07186730B2

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