참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Chloro-5-nitrobenzenesulfonyl chloride | HCID 20630 | — |
| 반응물 | 4-(1-Adamantanyl)-2-methylaniline hydrochloride | HCID 16376269 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N-(4-(1-adamantyl)-2-methylphenyl)-2-chloro-5-nitrobenzenesulfonamide | HCID 9955931 | 36.2% |
반응 단계
To 5 mL of a tetrahydrofuran solution comprising 250 mg of 4-(1-adamantyl)-2-methylaniline hydrochloride and 200 mg of triethylamine, 5 mL of a tetrahydrofuran solution comprising 230 mg of 2-chloro-5-nitrobenzenesulfonylchloride was dropwise added, followed by stirring at about 40° C. for about 7 hours. After the mixture was left to stand for cooling, water was added thereto, extraction with chloroform, drying over salt cake and concentration under reduced pressure were carried out to obtain crude crystals. The crude crystals were recrystalized from ether to obtain 150 mg of N-(4-(1-adamantyl)-2-methylphenyl)-2-chloro-5-nitrobenzenesulfonamide (Compound No. 48) having a melting point of 238° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07132546B2 |
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| 출처 데이터셋 | uspto-grants-2006_11 |
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| ORD ID | ord-777acafa4f66488789b044b218be0731 |
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| 출처 메모 | uspto-grants-2006_11 |
|---|