Methoxyacetyl chloride → 5-Methoxyacetylamino-2,4,6-triiodoisophthalic acid (2,3-diacetoxypropyl)amide chloride

HRID 1291972노트

반응식

HRID 1291972 반응식
[CH3:1][O:2][CH2:3][C:4]([Cl:6])=[O:5].[Cl-].[C:8]([O:11][CH:12]([CH2:30][O:31][C:32](=[O:34])[CH3:33])[CH2:13][NH:14][C:15](=[O:29])[C:16]1[C:24]([I:25])=[C:23]([NH2:26])[C:22]([I:27])=[C:18]([C:19]([OH:21])=[O:20])[C:17]=1[I:28])(=[O:10])[CH3:9]>O1CCOCC1>[Cl-:6].[C:8]([O:11][CH:12]([CH2:30][O:31][C:32](=[O:34])[CH3:33])[CH2:13][NH:14][C:15](=[O:29])[C:16]1[C:24]([I:25])=[C:23]([NH:26][C:4](=[O:5])[CH2:3][O:2][CH3:1])[C:22]([I:27])=[C:18]([C:19]([OH:21])=[O:20])[C:17]=1[I:28])(=[O:10])[CH3:9]

참가 물질

4

반응물 2

HCID 96623Methoxyacetyl chlorideHCID 867501615-amino-2,4,6-triiodisophthalic acid-N-(2,3-diacetoxypropyl)-amide-chloride

생성물 1

HCID 866509095-Methoxyacetylamino-2,4,6-triiodoisophthalic acid (2,3-diacetoxypropyl)amide chloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

24.7 g (150 mmol) of methoxyacetyl chloride is added at room temperature to a suspension of 73.4 g (100 mmol) of 5-amino-2,4,6-triiodisophthalic acid-N-(2,3-diacetoxypropyl)-amide-chloride (EP 0308364) in 500 ml of anhydrous dioxane, stirred with exclusion of moisture. The batch is refluxed for several hours, until no more feedstock can be detected according to thin-layer chromatography, then it is concentrated by evaporation, the residue is taken up in dichloromethane and shaken out with saturated aqueous sodium bicarbonate solution. After drying on anhydrous magnesium sulfate, the organic phase is concentrated by evaporation and the residue is recrystallized from ethyl acetate/tert-butyl methyl ether.

후처리

  1. temperatureThe batch is refluxed for several hours, until no more feedstock
  2. concentrationit is concentrated by evaporation
  3. stirringshaken out with saturated aqueous sodium bicarbonate solution
  4. dry with materialAfter drying on anhydrous magnesium sulfate
  5. concentrationthe organic phase is concentrated by evaporation
  6. customthe residue is recrystallized from ethyl acetate/tert-butyl methyl ether

출처 및 근거

ORD 기록
ord-7823c57ea137467eb0d95c00dd8d6479
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05756066

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