참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | 12-(tert-Butoxycarbonyl)-6,12-bis(benzyloxy)-7-oxo-6,12-diazadodecanenitrile | HCID 10324034 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 6,12-Bis(benzyloxy)-7-oxo-6,12-diazadodecanenitrile | HCID 10341465 | — |
반응 단계
Trifluoroacetic acid (25 mL) was slowly dripped into a solution of (4) (7.10 g, 13.93 mmol) in CH2Cl2 (150 mL) which had been cooled to 0° C. The solution was stirred at 0° C. for 30 minutes and at room temperature for 15 minutes. Solvent and excess TFA were removed by rotary evaporation, and the concentrate was cooled to 0° C., treated with saturated NaHCO3 (150 mL) and extracted with CH2Cl2 (4×80 mL). After solvent removal, the crude oil was purified by silica gel column chromatography with 1:1 hexane/EtOAc as the eluant, generating 4.6 g (81%) of (5) as an oil: NMR δ 1.40-190 (m, 8 H), 2.30 (t, 2 H, J=6), 2.40 (t, 2 H, J=6), 2.90 (t, 2 H, J=6), 3.63 (t, 2 H, J=6), 4.63 (s, 2 H), 4.75 (s, 2 H), 4.93 (br s, 1 H), 7.27 (s, 5 H), 7.33 (s, 5 H). Anal. (C24H31N3O3) C, H, N.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05322961 |
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| 출처 데이터셋 | uspto-grants-1994_06 |
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| ORD ID | ord-63b160e7ff22430e9ce2464bfd8afded |
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| 출처 메모 | uspto-grants-1994_06 |
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