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Potassium Carbonate → HCID 13321555, 화합물

HRID 1262817
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HRID 1262817 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 754301-Butanesulfonyl chlorideHCID 54703303HCID 54703303, 화합물

생성물 1

HCID 13321555HCID 13321555, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-24cef0660f6249f2a82fb59b0b613559
출처 데이터셋
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04454131

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