Hydrochloric Acid → HCID 13924322、化合物

HRID 2308613ノート

反応式

HRID 2308613 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[Cl:12][C:13]1[CH:14]=[C:15]([CH:19]=[C:20]([O:22][CH3:23])[N:21]=1)[C:16](Cl)=[O:17].Cl.CCCCCC.C(OC(=O)C)C>N1C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([S:8]([NH:11][C:16](=[O:17])[C:15]2[CH:19]=[C:20]([O:22][CH3:23])[N:21]=[C:13]([Cl:12])[CH:14]=2)(=[O:9])=[O:10])=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1202314-FluorobenzenesulfonamideHCID 27821252-chloro-6-methoxypyridine-4-carbonyl chlorideHCID 21226206Ethyl acetate hexane

生成物 1

HCID 13924322HCID 13924322、化合物収率 61%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

1.75 g (0.01 mol) of 4-fluorobenzenesulfonamide were dissolved in 30 ml of pyridine, and added dropwise by 2.06 g (0.01 mol) of 2-chloro-6-methoxyisonicotinoyl chloride at 0° C. to 5° C., followed by agitation for 2 hrs. at room temperature. After acidified by adding aqueous hydrochloric acid, the precipitate was extracted by ethyl acetate. The organic layer obtained was dried and them concentrated to precipitate crude crystals, which were recrystallized by n-hexane/ethylacetate to 2.1 g (yield: 61.0%) of N-(4-fluorophenylsulfonyl)-2-chloro-6-methoxy isonicotinamide as white crystal.

後処理

  1. customat room temperature
  2. extractionthe precipitate was extracted by ethyl acetate
  3. customThe organic layer obtained
  4. customwas dried
  5. concentrationthem concentrated
  6. customto precipitate crude crystals, which

出典と根拠

ORDレコード
ord-6be548f541cd42159275001e918b291d
出典データセット
uspto-grants-1987_09
特許番号
US04690934

反応ノート

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