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Triethylamine → HCID 20330247、化合物

HRID 2057753
ノート
印刷プレビュー

反応式

HRID 2057753 の反応式
[C:1](Cl)([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[O:2].[CH2:9]([O:11][C:12]1[CH:21]=[CH:20][C:15]([C:16]([NH:18][NH2:19])=[O:17])=[CH:14][CH:13]=1)[CH3:10].C(N(CC)CC)C>O1CCOCC1>[C:1]([NH:19][NH:18][C:16](=[O:17])[C:15]1[CH:20]=[CH:21][C:12]([O:11][CH2:9][CH3:10])=[CH:13][CH:14]=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

5

反応物 3

HCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 1435614-Ethoxybenzhydrazide

生成物 1

HCID 20330247HCID 20330247、化合物収率 90.7%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

29 g of ethoxalyl chloride are added, in the course of 30 minutes, to 36 g of 4-ethoxybenzhydrazide and 21.3 g of triethylamine in 360 ml of anhydrous dioxane, whilst keeping the temperature of the reaction medium at about 10° C. The stirring is continued (sic) for about two hours, whilst allowing the temperature to return to the ambient value. The reaction mixture is filtered, the filtrate is concentrated under reduced pressure (20 mm Hg, 50° C.) and the residue is stirred in the presence of 200 ml of isopropyl ether and then filtered off. After drying (20° C., 1 mm Hg), 50.8 g of 1-ethoxalyl-2-(4-ethoxybenzoyl)-hydrazine, which melts at 126° C. after a first melting at 120° C., are obtained. Yield: 90.7%.

後処理

  1. customat about 10° C
  2. customfor about two hours
  3. filtrationThe reaction mixture is filtered
  4. concentrationthe filtrate is concentrated under reduced pressure (20 mm Hg, 50° C.)
  5. filtrationfiltered off
  6. dry with materialAfter drying (20° C., 1 mm Hg), 50.8 g of 1-ethoxalyl-2-(4-ethoxybenzoyl)-hydrazine, which melts at 126° C. after a first melting at 120° C.
  7. customare obtained

出典と根拠

ORDレコード
ord-7f03a5e3ca5f432dab7702c73ea1aa18
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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