참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Sodium Azide | HCID 33557 | — |
| 반응물 | 6-Fluoro-2,3-dihydro-4H-1-benzothiopyran-4-one | HCID 2737521 | — |
| 생성물 | HCID 22036759 | HCID 22036759 | 75.1% |
반응 단계
6-fluoro-2,3-dihydro-4H-1-benzothiopyran-4-one (100 mg, 0.54 mmol) was dissolved in acetic acid (0.5 mL, 1.1 eq), sodium azide (71.2 mg, 1.1 mmol) was added and mixture was heated to 50° C. Sulfuric acid (0.13 mL, 4.3 eq) was added slowly and stirred at 50° C. for 1.5 hours. Ice chips (150 mg) were added and a green solid precipitated, this was filtered, washed with water and dried to give 7-fluoro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one (80 mg, 24%). 1H NMR (CDCl3, 300 MHz): δ 7.77 (s-broad, 1H), 7.69 (t, 1H, J=7.3 Hz), 6.94–6.82 (m, 2H), 3.42 (t, 2H, J=7 Hz), 2.63 (t, 2H, J=6.7 Hz) ppm.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07183282B2 |
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| 출처 데이터셋 | uspto-grants-2007_02 |
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| ORD ID | ord-4358dfe3e8294feeac48817dfb4b5d82 |
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| 출처 메모 | uspto-grants-2007_02 |
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