Ethanol → 2-Naphthohydrazide

HRID 2176344

반응식

HRID 2176344 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([O:13]C)=O.C(O)C.O.[NH2:19][NH2:20]>O>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([NH:19][NH2:20])=[O:13]

참가 물질

5

반응물 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 137605Methyl 2-naphthoate

생성물 1

HCID 1234852-Naphthohydrazide수율 88%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

First, 5.0 g of methyl 2-naphthoate and 20 mL of ethanol were put in a four-neck flask, and stirred. Then, 5 mL of hydrazine monohydrate (NH2NH2.H2O) was added to this mixture, and heated and stirred at 80° C. for 5 hours to be reacted. After the reaction, the solution was added to 100 mL of water, whereby a solid was precipitated. The resulting suspension was subjected to suction filtration to give a solid. This solid was recrystallized from a mixed solvent of chloroform and hexane, so that 4.4 g of 2-naphthohydrazide was prepared as a white solid with a yield of 88%. The synthetic scheme of Step 1 is shown by (a-12).

후처리

  1. temperatureheated
  2. stirringstirred at 80° C. for 5 hours
  3. customto be reacted
  4. customAfter the reaction
  5. customwas precipitated
  6. filtrationThe resulting suspension was subjected to suction filtration
  7. customto give a solid
  8. customThis solid was recrystallized from a mixed solvent of chloroform and hexane, so that 4.4 g of 2-naphthohydrazide
  9. customwas prepared as a white solid with a yield of 88%

출처 및 근거

ORD 기록
ord-f3b4d04564494160a8e6a4bf159034bc
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09065061B2

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