참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Sodium borohydride | HCID 4311764 | — |
| 반응물 | 2-(4-Fluorophenyl)-2H-1,4-benzothiazin-3(4H)-one | HCID 13690761 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-(4-fluorophenyl)-3,4-dihydro-2H-1,4-benzothiazine | HCID 18984416 | 91.2% |
반응 단계
To a mixture of 2-(4-fluorophenyl)-3-oxo-3,4-dihydro-2H-1,4-benzothiazine (4.0 g), sodium borohydride (2.91 g) and tetrahydrofuran (100 ml) is added dropwise with stirring boron trifluoride etherate complex (12. 5 ml) at room temperature, and the mixture is refluxed for 1.5 hour. After cooling, to the mixture is added dropwise 10% hydrochloric acid (35 ml), and the mixture is further refluxed for one hour. The reaction mixture is poured into ice water and made alkaline with potassium carbonate and extracted with ethyl acetate. The ethyl acetate layer is washed, dried and distilled to remove the solvent. The residue is recrystallized from isopropyl ether to give 2-(4-fluorophenyl)-3,4-dihydro-2H-1,4-benzothiazine (3.45 g, yield 91%) as crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05246929 |
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| 출처 데이터셋 | uspto-grants-1993_09 |
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| ORD ID | ord-ac2c06d7cbfb4525b6d01a68903c4d4b |
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| 출처 메모 | uspto-grants-1993_09 |
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