참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Formic Acid | HCID 284 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Chlorosulfonyl isocyanate | HCID 70918 | — |
| 반응물 | 2-Amino-6-bromonaphthalene | HCID 348404 | — |
| 용매 | Benzene | HCID 241 | — |
| 생성물 | 2-Bromo-6-(sulfamoylamino)naphthalene | HCID 22559043 | — |
반응 단계
A solution of chlorosulfonyl isocyanate (870 μl, WAKO) in benzene (10 ml) was added dropwise with formic acid (377 μl, WAKO) under ice cooling, warmed to room temperature, stirred and for 19.5 hours, then warmed to 40° C., and further stirred for 4 hours. The reaction mixture was added dropwise with a solution of 2-amino-6-bromonaphthalene (443 mg) in benzene (5 ml) under ice cooling, warmed to room temperature, and stirred 21.5 hours. The reaction mixture was filtered to obtain solid, and the solid was added with ethyl acetate, mixed and filtered again. The solvent of the filtrate was evaporated under reduced pressure. The residue was purified by column chromatography (Quad, hexane:ethyl acetate=2:1) to obtain the title compound (Intermediate 66, 158 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07470807B2 |
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| 출처 데이터셋 | uspto-grants-2008_12 |
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| ORD ID | ord-439009b9cbc64135ae37ed1c7f5f3d8d |
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| 출처 메모 | uspto-grants-2008_12 |
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