참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | 2-(4-Oxopentyl)-1H-isoindole-1,3(2H)-dione | HCID 236270 | — |
| 반응물 | 4-(4-Fluorobenzoyl)aminophenylhydrazine | HCID 11831684 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | N-[2-methyl-3-(2-phthalimidylethyl)-1H-indol-5-yl]-4-fluoro-benzamide | HCID 23290476 | 6.6% |
반응 단계
To a solution of 5.33 gm (21.7 mMol) 4-(4-fluorobenzoyl)aminophenylhydrazine and 5.03 gm (21.8 mMol) 5-phthalimidyl-2-pentanone in 100 mL ethanol were added 2 mL concentrated hydrochloric acid and the reaction mixture was heated at 80° C. for 14 hours. To the reaction mixture were then added an additional 3 mL concentrated hydrochloric acid and heating continued for an additional 6 hours. The reaction mixture was then cooled to 0° C. and 100 mL hexane were slowly added. The solid which formed was filtered and washed with hexane and provided, after drying, 6.67 gm of the desired compound. The mother liquor was concentrated under reduced pressure and then subjected to silica gel chromatography, eluting with 1:1 hexane:ethyl acetate. Fractions containing product were combined and concentrated under reduced pressure to provide an additional 0.63 gm of product. Overall yield was 7.3 gm (76%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05942536 |
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| 출처 데이터셋 | uspto-grants-1999_08 |
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| ORD ID | ord-819c94266a2841929f7934dcc8ce59c6 |
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| 출처 메모 | uspto-grants-1999_08 |
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