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Water → 68281-27-6

HRID 1448970
ノート
印刷プレビュー

反応式

HRID 1448970 の反応式
CC(C)=[O:3].OS(O)(=O)=O.O=[Cr](=O)=O.[OH:14][CH2:15][C:16]1([CH3:26])[O:21][C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=2[O:18][CH2:17]1.C(O)(C)C.O>CC(C)=O>[CH3:26][C:16]1([C:15]([OH:3])=[O:14])[O:21][C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=2[O:18][CH2:17]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 3776IsopropanolHCID 3778286(2-Methyl-2,3-dihydro-1,4-benzodioxin-2-yl)methanolHCID 131709961Jones' reagent

生成物 1

HCID 1263753668281-27-6

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Jones' reagent (33.3 ml.) was added dropwise to a stirred solution of 2-hydroxymethyl-2-methyl-1,4-benzodioxan (5 g.) in acetone (300 ml.) at 5° C., then the reaction was allowed to attain room temperature. Isopropanol (10 ml.) was then added followed by water (200 ml.), the solution extracted with chloroform and the extracts evaporated in vacuo. The residual oil was taken up in chloroform (200 ml.) then extracted with dilute sodium bicarbonate solution and the aqueous phase further washed with chloroform. The aqueous phase was then acidified with hydrochloric acid, extracted with chloroform, the combined extracts washed with water, dried (MgSO4) and evaporated in vacuo ti give 2-methyl-1,4-benzodioxan-2-carboxylic acid (1.7 g.). A sample was recrystallized from toluene, m.p. 133°-134° C.

後処理

  1. customto attain room temperature
  2. extractionthe solution extracted with chloroform
  3. customthe extracts evaporated in vacuo
  4. extractionthen extracted with dilute sodium bicarbonate solution
  5. washthe aqueous phase further washed with chloroform
  6. extractionextracted with chloroform
  7. washthe combined extracts washed with water
  8. dry with materialdried (MgSO4)
  9. customevaporated in vacuo ti

出典と根拠

ORDレコード
ord-d563cede87794726a093147db6fd5851
出典データセット
uspto-grants-1980_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04188390

反応ノート

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