Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 20-{3-[N-(4-methylhexahydrophthalimido)amino]-3-oxopropyl}-2,2,4,4-tetramethyl-7-oxa-3,20-diazadispiro[5.1.11.2]heneicosane-21-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Pentane | HCID 8003 | — |
| 반응물 | Hexahydro-4-methylphthalic anhydride | HCID 86876 | — |
| 반응물 | 20-(3-Hydrazino-3-oxopropyl)-2,2,4,4-tetramethyl-7-oxa-3,20-diazadispiro[5.1.11.2]heneicosane-21-one | HCID 18963138 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | 20-{3-[N-(4-methylhexahydrophthalimido)amino]-3-oxopropyl}-2,2,4,4-tetramethyl-7-oxa-3,20-diazadispiro[5.1.11.2]heneicosane-21-one | HCID 18963141 | — |
반응 단계
The hydrazide of Example 1, 13.5 g (0.03 mole), was added to 225 ml xylene at 75° C. Added dropwise to this was 4-methylhexahydrophthalic anhydride, 5.1 g (0.03 mole) in 25 ml xylene. The apparatus was fitted with a Dean Stark water separation assembly and the reaction mixture was heated to reflux for 4 hours with azeotropic removal of water as it formed. The xylenes were stripped using aspirator vacuum and the residual sticky solid was slurried with 300 ml pentane. The solid was filtered and dried for 2 hours on the filter funnel. The white solid product weighed 11.7 g and had a melting range of 210°-212° C. The infrared spectrum (mull) showed two carbonyl bands at 1690 and 1730 cm-1.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05352719 |
| 출처 데이터셋 | uspto-grants-1994_10 |
| ORD ID | ord-1ce6e273f96b447ca991dee7f0f7384c |
| 출처 메모 | uspto-grants-1994_10 |