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Potassium Carbonate → HCID 13321555、化合物

HRID 1262817
ノート
印刷プレビュー

反応式

HRID 1262817 の反応式
[CH3:1][C:2]1[C:6]([OH:7])=[C:5]([C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9])[S:4][C:3]=1[C:14]([O:16][CH:17]([CH3:19])[CH3:18])=[O:15].O1CCOCC1.C(=O)([O-])[O-].[K+].[K+].[CH2:32]([S:36](Cl)(=[O:38])=[O:37])[CH2:33][CH2:34][CH3:35]>CC(C)=O>[CH3:1][C:2]1[C:6]([O:7][S:36]([CH2:32][CH2:33][CH2:34][CH3:35])(=[O:38])=[O:37])=[C:5]([C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9])[S:4][C:3]=1[C:14]([O:16][CH:17]([CH3:19])[CH3:18])=[O:15]
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 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 754301-Butanesulfonyl chlorideHCID 54703303HCID 54703303、化合物

生成物 1

HCID 13321555HCID 13321555、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 2.3 g (8 mmol) of di-isopropyl 3-methyl-4-hydroxy-2,5-thiophene-dicarboxylate, 30 ml of dioxane, 60 ml of acetone, 1.6 g (120 mmol) of anhydrous potassium carbonate and 1.6 g (10 mmol) of butane-sulfonyl chloride was refluxed for about 10 hours. The mixture was then freed from dioxane and acetone by distillation in vacuo and then added with ethylether, washed with water, and dried with anhydrous magnessium sulfate. The solvent was removed by distillation and then recrystallization was effected from methanol to give 2.8 g (86%) of the desired white crystalline compound. m.p. 59°-61° C.

後処理

  1. temperaturewas refluxed for about 10 hours
  2. distillationThe mixture was then freed from dioxane and acetone by distillation in vacuo
  3. additionadded with ethylether
  4. washwashed with water
  5. dry with materialdried with anhydrous magnessium sulfate
  6. customThe solvent was removed by distillation
  7. customrecrystallization
  8. customto give 2.8 g (86%) of the desired white crystalline compound

出典と根拠

ORDレコード
ord-24cef0660f6249f2a82fb59b0b613559
出典データセット
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04454131

反応ノート

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