참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Monomethyl terephthalate | HCID 15513 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | Terephthalic acid monomethyl ester chloride diisopropylethylamine | HCID 86628494 | — |
반응 단계
A suspension of 1.997 kg (11.08 mol) of terephthalic acid monomethyl ester in 15.60 kg of 1,2-dimethoxyethane was stirred in a nitrogen atmosphere while being cooled at 10° C. To the suspension was added 400 mL (5.17 mol) of N,N-dimethylformamide and 1.323 kg (10.56 mol) of thionyl chloride in this order, and then the container was washed with 1.00 L of 1,2-dimethoxyethane. The suspension was stirred under heating at 60 to 73° C. for 1 hour and 2 minutes and then stirred while being cooled. 1.36 kg (10.52 mol) of N,N-diisopropylethylamine was added dropwise to the solution while cooling at 0° C., and the container was washed with 1.00 L of 1,2-dimethoxyethane. Then the reaction solution was stirred at 25° C., and the stirring was stopped 38 minutes after the internal temperature had reached 20° C. The reaction mixture was transferred into a plastic container, and 22.00 kg of “monomethyl terephthalate chloride/N,N-diisopropylethylamine” solution (terephthalic acid monomethyl ester chloride content: 1.84 kg) was obtained as a slightly tannish solution.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08530654B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-373df78e44d04ba793a20f1da510e383 |
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| 출처 메모 | uspto-grants-2013_09 |
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