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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 20330236、化合物

HRID 2057751
ノート
印刷プレビュー

反応式

HRID 2057751 の反応式
[C:1](Cl)([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[O:2].[CH3:9][C:10]1[CH:11]=[C:12]([CH:17]=[C:18]([CH3:20])[CH:19]=1)[C:13]([NH:15][NH2:16])=[O:14].C(N(CC)CC)C.O>O1CCOCC1>[C:1]([NH:16][NH:15][C:13](=[O:14])[C:12]1[CH:17]=[C:18]([CH3:20])[CH:19]=[C:10]([CH3:9])[CH:11]=1)([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[O:2]
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 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 38583463,5-Dimethylbenzohydrazide

生成物 1

HCID 20330236HCID 20330236、化合物収率 70.2%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

265 g of ethoxalyl chloride are added, in the course of one hour, to 316 g of 3,5-dimethylbenzhydrazide and 195 g of triethylamine in 1.58 liters of anhydrous dioxane, whilst keeping the temperature of the reaction medium at about 10°-12° C. The stirring is continued (sic) for about two hours. whilst allowing the temperature to return to the ambient value. The reaction mixture is then poured into seven liters of water, whilst stirring. The precipitate which has formed is filtered off, washed three times with one liter of water and then dried at 20° C. under a pressure of one millimeter of mercury. 357 g of 1-ethoxalyl-2-(3,5-dimethylbenzoyl)-hydrazine, which melts at 159° C., are obtained.

後処理

  1. customat about 10°-12° C
  2. customfor about two hours
  3. customThe precipitate which has formed
  4. filtrationis filtered off
  5. washwashed three times with one liter of water
  6. customdried at 20° C. under a pressure of one millimeter of mercury

出典と根拠

ORDレコード
ord-2ff9f955193244c7875382a7bc874e96
出典データセット
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04212867

反応ノート

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