참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | O-Toluidine | HCID 7242 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Isatoic Anhydride | HCID 8359 | — |
| 반응물 | Acetanthranil | HCID 68236 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | Methaqualone | HCID 6292 | 64% |
반응 단계
The isatoic anhydride and acetic anhydride were reacted under the condition described for the preparation of 2-methyl-4H-3,1-benzoxazine-4-one. The pyridine was distilled from the reaction mixture under reduced pressure. The crude reaction product was taken up in 100 ml of o-xylene and placed in a 200 ml one-necked flask equipped with a Dean-Stark trap and a reflux condenser. The o-toluidine was added to the xylene solution. The reaction mixture was heated to reflux for 4 hours. 1.8 ml of water was collected in the Dean-Stark trap. The xylene was removed from the reaction product by distillation under reduced pressure. The resulting residue was crystallized twice from methanol to give 16 parts (64% yield) of 2-methyl-3-(o-tolyl)-quinazoline-4 (3H)-one with m.p. 113°-115° C. The reaction product was characterized by melting point, IR and NMR.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US03989698 |
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| 출처 데이터셋 | uspto-grants-1976_11 |
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| ORD ID | ord-4e79fd1e4e6543018bae9e7379e09792 |
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| 출처 메모 | uspto-grants-1976_11 |
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