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Triethylamine → HCID 20330247, 화합물

HRID 2057753
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HRID 2057753 반응식
[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]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 1435614-Ethoxybenzhydrazide

생성물 1

HCID 20330247HCID 20330247, 화합물수율 90.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-7f03a5e3ca5f432dab7702c73ea1aa18
출처 데이터셋
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04212867

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