Sodium Hydroxide → HCID 178465676, 화합물

HRID 128408

반응식

HRID 128408 반응식
Cl.[C:2]([NH2:5])(=[NH:4])[CH3:3].[OH-].[Na+].[CH:8]([S:16](Cl)(=[O:18])=[O:17])=[CH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>CC(C)=O>[CH:8]([S:16]([NH:4][C:2](=[NH:5])[CH3:3])(=[O:18])=[O:17])=[CH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 67170Acetamidine monohydrochlorideHCID 107500Ethenesulfonyl chloride, 2-phenyl-

생성물 1

HCID 178465676HCID 178465676, 화합물수율 76%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A mixture of acetamidine hydrochloride (28.8 g., 0.15 mole) and 50% sodium hydroxide (12.0 g., 0.15 mole) in 150 ml. of acetone is stirred for a period of 10 min. to liberate the free base. A solution of styrylsulfonyl chloride (10.1 g., 0.05 mole) in 50 ml. of acetone is added dropwise to the mixture at a temperature of 20°-25° C. with stirring. After further stirring for 10 min., the mixture is concentrated under reduced pressure to remove acetone, the concentrate diluted with 200 ml. of water and acidified with 3 N hydrochloric acid to provide a precipitate. The precipitate is collected, dissolved in chloroform and the chloroform extract dried. Evaporation of the chloroform solvent under reduced pressure provides a white solid, m.p. 130°-134° C. which is crystallized from isopropyl acetate affording 8.5 g. (76% yield) of N-(STYRYLSULFONYL)ACETAMIDINE, m.p. 134.5°-137.0° C. (corr.).

후처리

  1. stirringAfter further stirring for 10 min.
  2. concentrationthe mixture is concentrated under reduced pressure
  3. customto remove acetone
  4. additionthe concentrate diluted with 200 ml
  5. customto provide a precipitate
  6. customThe precipitate is collected
  7. dissolutiondissolved in chloroform
  8. extractionthe chloroform extract
  9. customdried
  10. customEvaporation of the chloroform solvent under reduced pressure
  11. customprovides a white solid, m.p. 130°-134° C. which
  12. customis crystallized from isopropyl acetate affording 8.5 g

출처 및 근거

ORD 기록
ord-87102362e1fd4358a8c99927fc0420cb
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259482

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