Chromic Acid → HCID 13645870、化合物

HRID 1982267ノート

反応式

HRID 1982267 の反応式
[C:1]([O:4][CH2:5][CH:6]1[O:11][C:10]2[C:12]([Cl:19])=[C:13]([Cl:18])[CH:14]=[C:15]([CH:16]=[O:17])[C:9]=2[O:8][CH2:7]1)(=[O:3])[CH3:2].[Cr](O)(O)(=O)=[O:21]>CC(C)=O>[C:1]([O:4][CH2:5][CH:6]1[O:11][C:10]2[C:12]([Cl:19])=[C:13]([Cl:18])[CH:14]=[C:15]([C:16]([OH:21])=[O:17])[C:9]=2[O:8][CH2:7]1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 24425Chromic AcidHCID 13645808HCID 13645808、化合物

生成物 1

HCID 13645870HCID 13645870、化合物収率 93%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 1.03 g of 2-acetoxymethyl-7,8-dichloro-1,4-benzodioxane-5-carbaldehyde (Ia-a-39) in 70 ml of acetone is added 2 ml of 8N-chromic acid/sulfric acid. The mixture is stirred at room temperature for about 2.5 hours and then filtered after the confirmation by TLC that no starting material is remained. The filtrate is concentrated under reduced pressure to give a residue, which is extracted with dichloromethane. The organic layer is washed with water and evaporated to give 1.004 g (93%) of 2-acetoxymethyl-7,8-dichloro-1,4-benzodioxane-5-carboxylic acid (Ia-a-43: R3 '=Ac), which is recrystallized from dichloromethane/ether to yield crystals, m.p. 144°-145° C.

後処理

  1. filtrationfiltered after the confirmation by TLC that no starting material
  2. concentrationThe filtrate is concentrated under reduced pressure
  3. customto give a residue, which
  4. extractionis extracted with dichloromethane
  5. washThe organic layer is washed with water
  6. customevaporated

出典と根拠

ORDレコード
ord-90cae9718e6c4d91808bfef5a7b494d4
出典データセット
uspto-grants-1986_06
特許番号
US04595767

反応ノート

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