참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | Ethyl chloroformate | HCID 10928 | — |
| 반응물 | 9H-Pyrido(3,4-b)indole-3-carboxylic acid | HCID 173262 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | FG-7142 | HCID 4375 | — |
반응 단계
A suspension of 5 g of β-carbolin-3-carboxylic acid in a mixture of 900 ml of tetrahydrofuran and 3.6 ml of triethylamine is boiled under reflux for 15 minutes and cooled to room temperature. Freshly distilled ethyl chloroformate (2.5 ml), dissolved in 100 ml of tetrahydrofuran, is added dropwise with stirring over a period of 11/2 hours. After the reaction mixture has been stirred for an additional 30 minutes, a large excess of methylamine is added. Stirring is continued for one hour, whereafter the mixture is filtered and concentrated to approximately 50 ml under reduced pressure. Addition of water (250 ml) causes the amide to precipitate. The mixture is left at 5° C. overnight, filtered and dried at 60° C. for 15 hours. β-carbolin-3-carboxylic acid methylamide thus formed (4.1 g; 77%) is recrystallized from toluene. The melting point is 275° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04371536 |
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| 출처 데이터셋 | uspto-grants-1983_02 |
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| ORD ID | ord-5d82fec7f001468c831d74f44b829859 |
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| 출처 메모 | uspto-grants-1983_02 |
|---|