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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Methoxide → 2-[3-(2-propenyl)-6-fluoro-2(3H)-benzothiazolon-5-yl]-hexahydro-1H-[1,2,4]triazolo[1,2-a]pyridazine-1,3-dione

HRID 1761806
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HRID 1761806 반응식
[F:1][C:2]1[C:14]([NH:15][C:16]([N:18]2[CH2:23][CH2:22][CH2:21][CH2:20][N:19]2[C:24](OCC)=[O:25])=[O:17])=[CH:13][C:5]2[N:6]([CH2:10][CH:11]=[CH2:12])[C:7](=[O:9])[S:8][C:4]=2[CH:3]=1.C[O-].[Na+]>O>[CH2:10]([N:6]1[C:5]2[CH:13]=[C:14]([N:15]3[C:24](=[O:25])[N:19]4[CH2:20][CH2:21][CH2:22][CH2:23][N:18]4[C:16]3=[O:17])[C:2]([F:1])=[CH:3][C:4]=2[S:8][C:7]1=[O:9])[CH:11]=[CH2:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 14049866Ethyl 2-[6-fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-ylaminocarbonyl]-hexahydropyridazine-1-carboxylate

생성물 1

HCID 140498672-[3-(2-propenyl)-6-fluoro-2(3H)-benzothiazolon-5-yl]-hexahydro-1H-[1,2,4]triazolo[1,2-a]pyridazine-1,3-dione수율 10.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Ethyl 2-[6-fluoro-3-(2-propenyl)-2(3H)-benzothiazolon-5-ylaminocarbonyl]-hexahydropyridazine-1-carboxylate (1.55 g) was added to a methanolic solution (2.05 g) of 10% sodium methoxide, and the resultant mixture was heated under reflux for 1.5 hours and allowed to cool. Water was added thereto, and the mixture was extracted with ethyl acetate. The extract was washed with water, dried, concentrated and purified by silica gel thin layer chromatography with a mixture of ethyl acetate and hexane (1:1) as an eluent to give 2-[3-(2-propenyl)-6-fluoro-2(3H)-benzothiazolon-5-yl]-hexahydro-1H-[1,2,4]triazolo[1,2-a]pyridazine-1,3-dione (0.15 g). m.p., 199.5° C.

후처리

  1. temperatureunder reflux for 1.5 hours
  2. temperatureto cool
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with water
  5. customdried
  6. concentrationconcentrated
  7. custompurified by silica gel thin layer chromatography with a mixture of ethyl acetate and hexane (1:1) as an eluent

출처 및 근거

ORD 기록
ord-cb9d0991acba4a5a9f9d2acab3f8a9d3
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04828605

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