Chromic Acid → HCID 13645870, 화합물

HRID 1982267노트

반응식

HRID 1982267 반응식
[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]

참가 물질

4

반응물 2

HCID 24425Chromic AcidHCID 13645808HCID 13645808, 화합물

생성물 1

HCID 13645870HCID 13645870, 화합물수율 93%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-90cae9718e6c4d91808bfef5a7b494d4
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04595767

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