참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Nitro-o-anisic acid | HCID 75776 | — |
| 반응물 | 2-Amino-5-methoxybenzene-1-thiol | HCID 235509 | — |
| 용매 | Dichloromethane methanol | HCID 21226129 | — |
| 생성물 | 2-(2-Methoxy-4-nitrophenyl)-6-methoxybenzothiazole | HCID 67237195 | 84.2% |
반응 단계
A thoroughly mixed paste of 2-amino-5-methoxybenzenethiol (2.0 g, 12.88 mmol) and 2-methoxy-4-nitrobenzoic acid (2.54 g, 12.88 mmol) in trimethylsilylpolyphosphate (10 ml) was stirred and heated at 150° C. under an atmosphere of argon for 30 min. On cooling to room temperature, the reaction mixture was suspended in DCM/MeOH and an orange solid was collected by filtration. The filtrate was washed with 1 M HCl (2×50 ml), sat. NaHCO3 (2×50 ml), brine (70 ml) and dried (Na2SO4). The solvent was removed under reduced pressure to give a solid which was combined with that collected and recrystallised from AcOH to give the title compound (3.43 g, 83%) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08895313B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-d0507224f6004267a22b2c908592f5c8 |
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| 출처 메모 | uspto-grants-2014_11 |
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