Sodium Hydroxide → HCID 16781333、化合物

HRID 456588

反応式

HRID 456588 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 16781333HCID 16781333、化合物収率 100.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-6c474692bdbe4f82b3b6d1648d1a2bc8
出典データセット
uspto-grants-2007_03
特許番号
US07186730B2

関連ノート

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