1,4-Dioxane → HCID 54005561, compound

HRID 2254060Notes

Reaction equation

HRID 2254060 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][NH:10][C:11]1[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][C:12]=1[C:13]([NH:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[O:14].[O:28]1CCOC[CH2:29]1>>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][N:10]1[C:11]2[C:12](=[CH:22][C:23]([O:26][CH3:27])=[CH:24][CH:25]=2)[C:13](=[O:14])[N:15]([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:29]1=[O:28]

Participants

3

Reactant 2

HCID 312751,4-DioxaneHCID 54491738HCID 54491738, compound

Product 1

HCID 54005561HCID 54005561, compound

Conditions

Temperature
140 °C

Procedure

Into 10 ml of dioxane were dissolved 5.2 g of ethyl (2-((2,4-dichlorophenyl)methyl)amino-5-methoxybenzoyl)aminoacetate and 6.2 g of N,N'-carbonyldiimidazole, and the solution was heated to 140° to 150° C. After distilled off dioxane, the mixture was further heated for 15 minutes at 140° C. After cooling, ethanol was added and the crystalline substances were collected by filtration. They were recrystallized from ethanol to obtain 2,8 g of title compound. m.p. 167°-168° C.

Workup

  1. temperaturethe solution was heated to 140° to 150° C
  2. distillationAfter distilled off dioxane
  3. temperatureAfter cooling
  4. additionethanol was added
  5. filtrationthe crystalline substances were collected by filtration
  6. customThey were recrystallized from ethanol

Sources & evidence

ORD record
ord-313bc59c2b6d406485f1f99830aade50
Source dataset
uspto-grants-1993_08
Patent number
US05234928

Reaction notes

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