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Citric Acid → HCID 19083157、化合物

HRID 1734418
ノート
印刷プレビュー

反応式

HRID 1734418 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 19083157HCID 19083157、化合物収率 90%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-475507eaf6f8497fb6061c59e2476c90
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05534481

反応ノート

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