참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Water | HCID 962 | — |
| 반응물 | Methyl (2-amino-4-chloro-5-fluorophenyl)acetate | HCID 10900080 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 6-Chloro-5-fluoroindolin-2-one | HCID 9794083 | — |
반응 단계
Compound (III) is obtained by cyclizing (II) with an acid as shown in step [b] of Scheme 1. Compound (II) is dissolved in a mixture of an acid and a cosolvent, preferably the acid is glacial acetic acid in which instance the preferred cosolvent is water or the acid is hydrochloric acid in which instance the preferred cosolvent is methylene chloride. With acetic acid the ratio of the acid and cosolvent mixture ranges from 2:1 to pure acetic acid respectively, the preferred ratio being 6:1. With HCl, much less acid is required, preferably 1:4 3N HCl to CH2Cl2. Once compound (II) is dissolved, the reaction mixture is stirred at ambient temperature for from 6 to 7 hours to produce 5-fluoro-6-chlorooxindole (III). Compound (III) is readily purified by recrystallization from ethyl acetate to yield an off-white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05166401 |
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| 출처 데이터셋 | uspto-grants-1992_11 |
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| ORD ID | ord-f6e926db4fe440bcbe8c2c714bdbecf2 |
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| 출처 메모 | uspto-grants-1992_11 |
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