참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Acetamidine monohydrochloride | HCID 67170 | — |
| 반응물 | Ethenesulfonyl chloride, 2-phenyl- | HCID 107500 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | HCID 178465676 | HCID 178465676 | 76% |
반응 단계
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.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04259482 |
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| 출처 데이터셋 | uspto-grants-1981_03 |
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| ORD ID | ord-87102362e1fd4358a8c99927fc0420cb |
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| 출처 메모 | uspto-grants-1981_03 |
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