Hydrochloric Acid → HCID 13924322, 화합물

HRID 2308613노트

반응식

HRID 2308613 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 13924322HCID 13924322, 화합물수율 61%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6be548f541cd42159275001e918b291d
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04690934

반응 노트

불러오는 중…