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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Cyclopropyl methyl ketone → 1-Cyclopropyl-3-(3-pyridazinyl)-1,3-propanedione

HRID 1076689
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반응식

HRID 1076689 반응식
C(O[C:4]([C:6]1[N:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:5])C.[CH:12]1([C:15]([CH3:17])=[O:16])[CH2:14][CH2:13]1.C[O-].[Na+]>C1C=CC=CC=1>[CH:12]1([C:15](=[O:16])[CH2:17][C:4]([C:6]2[N:7]=[N:8][CH:9]=[CH:10][CH:11]=2)=[O:5])[CH2:14][CH2:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 13004Cyclopropyl methyl ketoneHCID 10942334Sodium MethoxideHCID 14452007Ethyl pyridazine-3-carboxylate

생성물 1

HCID 123605611-Cyclopropyl-3-(3-pyridazinyl)-1,3-propanedione

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A stirred mixture of 4.0 g. of ethyl-3-pyridazinecarboxylate, 4.4 g. of cyclopropylmethyl ketone and 1.6 g. of sodium methoxide in 100 ml. of benzene is heated under reflux for 5 hours. The mixture is diluted with 300 ml. of water and the benzene phase is separated. The aqueous mixture is made weakly acidic with dilute hydrochloric acid and extracted with chloroform. The chloroform solution is dried over magnesium sulfate and concentrated under reduced pressure to yield straw-colored crystals which are recrystallized from acetonitrile to give cream-colored crystals, melting point 85°-87°C.

후처리

  1. additionA stirred mixture of 4.0 g
  2. temperatureunder reflux for 5 hours
  3. additionThe mixture is diluted with 300 ml
  4. customof water and the benzene phase is separated
  5. extractionextracted with chloroform
  6. dry with materialThe chloroform solution is dried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto yield straw-colored crystals which
  9. customare recrystallized from acetonitrile
  10. customto give cream-colored crystals, melting point 85°-87°C.

출처 및 근거

ORD 기록
ord-dee5d170abcf4ec79a490c1160d16b96
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03957805

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