참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cyclohexylamine hydrochloride | HCID 2723770 | — |
| 반응물 | (2-Methylphenyl)cyanamide | HCID 10261129 | — |
| 용매 | Chlorobenzene | HCID 7964 | — |
| 생성물 | HCID 178424369 | HCID 178424369 | 26.5% |
반응 단계
A suspension of cyclohexylamine hydrochloride (310 mg, 2.28 mmol) and (2-methylphenyl)cyanamide (365 mg, 2.76 mmol) in dry chlorobenzene was heated at 125°-135° for 4 hrs. The solvent was evaporated in vacuo with heating, and the residue partitioned between CH2Cl2 and 20-8 ml 10% HCl. The aqueous extracts were made alkaline to pH 9-9.5, and the white precipitate collected after standing at 4° C. overnight. Two recrystallizations from EtOH/H2O gave 140 mg (22%) of white needles, mp 145°-146°, 1H (CD3OD) 1.149-2.054 (m, 10 H), 2.164 (s, 3 H), 3.50 (m, 1 H), 6.875 (d, 1H, J=7.5 Hz), 6.968 (t, 1H, J=7.5 Hz), 7.118 (t, 1H, J=7.5 Hz), 7.177 (d, 1H, J=7.5 Hz). Anal. Calcd for C14H21N3 : C, 72.69; H, 9.15; N, 18.16. Found: C, 72.72; H, 9.24; N, 18.18.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05604228 |
|---|
| 출처 데이터셋 | uspto-grants-1997_02 |
|---|
| ORD ID | ord-dcaae0ecc5004d0fb31968c4b43b6a9f |
|---|
| 출처 메모 | uspto-grants-1997_02 |
|---|