Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 261302생성일: 2026년 10월 26일
beta,beta'-Thiodipropionitrile → Acetamide, N-(2-(2-(2-cyano-4,6-dinitrophenyl)diazenyl)-5-(diethylamino)phenyl)-
https://huagongshe.com/reaction/261302
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | beta,beta'-Thiodipropionitrile | HCID 8151 | — |
| 반응물 | Sodium Cyanide | HCID 8929 | — |
| 반응물 | Acetamide, N-[2-[2-(2-bromo-4,6-dinitrophenyl)diazenyl]-5-(diethylamino)phenyl]- | HCID 104287 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Acetamide, N-(2-(2-(2-cyano-4,6-dinitrophenyl)diazenyl)-5-(diethylamino)phenyl)- | HCID 90383 | — |
반응 단계
Into a reactor there are introduced 765 parts of bis (β-cyanoethyl) sulfide, followed by 14.35 parts of cuprous bromide. On heating to 60° C. with continuous stirring, a brownish-yellow solution of the copper complex is obtained. 95.8 parts of 3-acetamido-4-(2'bromo-4',6'-dinitrophenylazo)-N,N-diethylaniline are added, and the temperature is raised to 115° C. Raising the temperature to 115° C. causes the compound to completely dissolve. At ths temperature, a solution of 10.8 parts of sodium cyanide in 40 parts of water is introduced into the reactor during a period of 20 minutes, allowing the steam to escape. Stirring is continued for a further 20 to 30 minutes while verifying by thin layer chromatography that the starting organic bromo-derivative is absent. The reaction mass is cooled to 30°-35° C., which causes crystallization of the dyestuff. The resultant product is filtered off, washed with water to displace the solvent contained in the paste, and dried. 80.2 parts of 3 -acetamido-4-(2'cyano-4',6'-dinitro-phenylazo)-N,N-diethylaniline are obtained. The titre (purity) of this product is 98.5% and it contains a copper concentration of less than 3000 parts per million. The wash water is introduced into a decanter, and the organic solvent part is withdrawn and reunited with the fraction of solvent obtained during filtration. There are thus recovered 720 parts of bis(β-cyanoethyl) sulfide which contain 4.35 parts of the cyanoazo dyestuff (giving an overall balance of the reaction of 98%) and 5.75 parts of copper (which corresponds to a recovery of 91% of the initial copper complex.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04165297 |
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| 출처 데이터셋 | uspto-grants-1979_08 |
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| ORD ID | ord-0776cbb3f98d4a2b9b06faee814feb4b |
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| 출처 메모 | uspto-grants-1979_08 |
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