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Citric Acid → HCID 19083157, 화합물

HRID 1378928
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HRID 1378928 반응식
[H-].[Na+].[CH:3]1([CH2:6][OH:7])[CH2:5][CH2:4]1.F[C:9]1[C:10]2[C:14]([CH:15]=[CH:16][CH:17]=1)=[N:13][N:12]([CH3:18])[C:11]=2[S:19]([NH2:22])(=[O:21])=[O:20].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CS(C)=O>[CH:3]1([CH2:6][O:7][C:9]2[C:10]3[C:14]([CH:15]=[CH:16][CH:17]=2)=[N:13][N:12]([CH3:18])[C:11]=3[S:19]([NH2:22])(=[O:21])=[O:20])[CH2:5][CH2:4]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 311Citric AcidHCID 24758Sodium hydrideHCID 75644CyclopropanemethanolHCID 190831614-fluoro-2-methyl-2H-indazole-3-sulfonamide

생성물 1

HCID 19083157HCID 19083157, 화합물수율 90%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

2.8 g (70 mmol) of 60% sodium hydride was suspended in 50 ml of DMSO, and 6 g (83 mmol) of cyclopropane methanol was dropwise added thereto. The mixture was stirred at room temperature for one hour, and then 5.4 g (24 mmol) of 4-fluoro-2-methyl-2H-indazole-3-sulfonamide was added thereto. The mixture was stirred at 130° C. for 3 hours. After the reaction, the mixture was poured into ice water, acidified with citric acid and extracted with ethyl acetate. The organic layer was washed with water and then concentrated. Formed crystals were collected by filtration, washed with IPE and then dried to obtain 5.8 g (yield: 90%) of the desired product. Melting point: 139°-141° C.

후처리

  1. stirringThe mixture was stirred at 130° C. for 3 hours
  2. customAfter the reaction
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. concentrationconcentrated
  6. customFormed crystals
  7. filtrationwere collected by filtration
  8. washwashed with IPE
  9. customdried

출처 및 근거

ORD 기록
ord-084e2a3a6a5f48fa9536dd58c715d186
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05670452

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