참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trimethylsilylacetylene | HCID 66111 | — |
| 반응물 | HCID 67938489 | HCID 67938489 | — |
| 용매 | Toluene triethylamine | HCID 22504574 | — |
| 생성물 | HCID 86739598 | HCID 86739598 | 70.5% |
반응 단계
A slurry of 3.00 g (9.02 mmoles) of 6-bromophenyl)benzimidazoquinazoline, 100 mg of diacetatobis(triphenylphosphine)palladium[II] in 150 ml of 2:1 triethylamine-toluene was heated to 100° C. under argon and then treated with dropwise addition of 1.57 g (16.0 mmoles) of ethynyltrimethylsilane. After 3.5 hours, the mixture was cooled and filtered. The filtrate was diluted with 100 ml of ether, washed with 200 ml each of 5% hydrochloric acid and water, and then dried over magnesium sulfate. Concentrating the clear solution yielded a solid mass which upon trituration with hexane gave 2.21 g (56.5 mmoles, 70.5%) of 6-(m-trimethylsilylethynylphenyl)benzimidazoquinazoline: ir (KBr): 3077 (medium, sharp, C-H), 2960 (medium, sharp, SiCH), 2155 (strong, sharp, C≡C), 1621, 1587 (v. strong, sharp, C=N), 1524, 1456, 1441, 1355, 1325 (strong, sharp, C=C), 1247 (v. strong, sharp, Si--C) and 844 cm-1 (v. strong, broad, Si--C bending); mass spectrum (70 ev) m/e 391.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04465833 |
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| 출처 데이터셋 | uspto-grants-1984_08 |
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| ORD ID | ord-c83b308a3bc24421aaceda338e3e5340 |
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| 출처 메모 | uspto-grants-1984_08 |
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