Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Formaldehyde → 3-Oxa-1-azaspiro[4.5]decane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | (1-Aminocyclohexyl)methanol | HCID 409153 | — |
| 용매 | Methanol--water (1/1) | HCID 22242641 | — |
| 생성물 | 3-Oxa-1-azaspiro[4.5]decane | HCID 22622870 | 83% |
반응 단계
To a 500 mL flask containing 1-amino-cyclohexylmethanol (135 g, 1.05 mol) and methanol (50 mL) is added methyl formcel (53 mL of 55% formaldehyde in methanol/water, 1.06 mol) dropwise over a 1 hour period. During the addition, the stirred solution is warmed gently from room temperature to 37° C. After the addition is completed, the mixture is allowed to stir overnight at room temperature. The clear, colorless reaction mixture is stripped on a rotary evaporator (50° C./29″ vacuum). The resulting oil is distilled under vacuum giving a clear, colorless, mobile liquid with a boiling point of 43° C./0.8 torr. A total of 123.4 g is collected (83% yield). A GC analysis indicates 95.6% purity.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09187436B2 |
| 출처 데이터셋 | uspto-grants-2015_11 |
| ORD ID | ord-a1256313b3864d9d8caac7c4b411e923 |
| 출처 메모 | uspto-grants-2015_11 |