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Ethanol → Ethyl 2-{[(3-iodophenyl)amino]carbonyl}hydrazinecarboxylate

HRID 857133
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인쇄 미리보기

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HRID 857133 반응식
[C:1]([O:5][CH2:6][CH3:7])(=[O:4])[NH:2][NH2:3].[I:8][C:9]1[CH:10]=[C:11]([N:15]=[C:16]=[O:17])[CH:12]=[CH:13][CH:14]=1.C(O)C>ClCCl>[I:8][C:9]1[CH:10]=[C:11]([NH:15][C:16]([NH:3][NH:2][C:1]([O:5][CH2:6][CH3:7])=[O:4])=[O:17])[CH:12]=[CH:13][CH:14]=1
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참가 물질

5

반응물 3

HCID 702EthanolHCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 44990001-Iodo-3-isocyanatobenzene

생성물 1

HCID 21867116Ethyl 2-{[(3-iodophenyl)amino]carbonyl}hydrazinecarboxylate수율 99.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
20 °C

실험 절차

A solution of ethyl carbazate (1.25 g) in dichloromethane (20 ml) was treated with 3-iodophenylisocyanate (1.7 g) at 0° C. The reaction mixture was allowed to warm to 20° C. and stirred for 2 h. Ethanol (2 ml) was added and the mixture was stirred for 0.5 h. The solvents were removed under reduced pressure and the residue was triturated in diethyl ether. The white solid was collected by filtration to give the title compound (2.4 g). LCMS RT=2.81 min

후처리

  1. stirringthe mixture was stirred for 0.5 h
  2. customThe solvents were removed under reduced pressure
  3. customthe residue was triturated in diethyl ether
  4. filtrationThe white solid was collected by filtration

출처 및 근거

ORD 기록
ord-e603dd6d9b484b44a170870b3bcfc6ce
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07144908B2

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