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Ethyl formate → HCID 57144783, 화합물

HRID 569911
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HRID 569911 반응식
[CH3:1][N:2]1[C:6]2[CH2:7][CH2:8][CH2:9][CH2:10][C:11](=[O:12])[C:5]=2[CH:4]=[N:3]1.[H-].[Na+].[CH:15](OCC)=[O:16]>C(O)C.O1CCCC1>[OH:16][CH:15]=[C:10]1[C:11](=[O:12])[C:5]2[CH:4]=[N:3][N:2]([CH3:1])[C:6]=2[CH2:7][CH2:8][CH2:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 201465961-methyl-1H,4H,5H,6H,7H,8H-cyclohepta[c]pyrazol-4-one

생성물 1

HCID 57144783HCID 57144783, 화합물

시약·촉매·용매 2

HCID 702Ethanol촉매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 7 grams of 5,6,7,8-tetrahydro-1-methyl4(1H)-cycloheptapyrazolone, 2.3 grams of sodium hydride (97%), 12 ml of ethyl formate, 2 drops of ethanol and 100 ml of tetrahydrofuran was heated at reflux for 3 hours. The mixture was then cooled and partitioned between water and ether. The aqueous layer was washed once with ether and acidified to a pH of 5 with 1 N hydrochloric acid. The white precipitate which formed was separated by filtration and dried to give 5,6,7,8-tetrahydro-5-hydroxymethylene-1-methyl-4(1H)-cycloheptapyrazolone as a cream colored powder melting at about 133°-135° C.

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후처리

  1. temperaturewas heated
  2. temperatureat reflux for 3 hours
  3. temperatureThe mixture was then cooled
  4. custompartitioned between water and ether
  5. washThe aqueous layer was washed once with ether
  6. customThe white precipitate which formed
  7. customwas separated by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-8bb048309e6e435f9e9ef975be0f0aac
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04734430

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