Hydrochloric Acid → 1405433-13-7

HRID 1777744노트

반응식

HRID 1777744 반응식
Cl.[NH:2]([CH2:4][C:5]([O:7]CC)=[O:6])[NH2:3].CN(C)/[CH:12]=[CH:13]/[C:14]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=O.C([O-])([O-])=O.[K+].[K+].Cl>CCO.CC(=O)OCC>[C:16]1([C:14]2[N:2]([CH2:4][C:5]([OH:7])=[O:6])[N:3]=[CH:12][CH:13]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 5398495(E)-3-Dimethylamino-1-phenyl-propenoneHCID 11593468Acetic acid, 2-hydrazinyl-, ethyl ester, hydrochloride (1:1)

생성물 1

HCID 216451761405433-13-7수율 63.6%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

To a solution of ethyl hydrazinoacetate hydrochloride (866 mg) in EtOH (20 mL) was added (E)-3-(dimethylamino)-1-phenylprop-2-en-1-one (981 mg) and K2CO3 (774 mg). The reaction mixture was stirred at 80° C. for 20 h, cooled down and the pH was brought to 2-3 by adding 1M HCl. EA was added and the phases were separated. The org. layer was washed with brine, dried (Na2SO4) and evaporated in vacuo to afford 720 mg of white solid. LC-MS (B): tR=0.63 min; [M+H]+: 203.43.

후처리

  1. temperaturecooled down
  2. customthe phases were separated
  3. washlayer was washed with brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-7462d79b031f4d2aa6504aebb6d92cef
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09266876B2

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