반응식
C([NH:3][C:4]([NH:6][CH:7]1[CH2:9]C1)=[NH:5])#N.[ClH:10].N1CC[O:14][CH2:13][CH2:12]1>C(O)(C)C>[ClH:10].[N:6]1([C:4](=[NH:5])[NH2:3])[CH2:7][CH2:9][O:14][CH2:13][CH2:12]1참가 물질
4
반응 조건
- 온도
- 160 °C
실험 절차
A mixture of 4.0 g (32.3 mmoles) of N-cyano-N'-cyclopropylguanidine and 3.98 g (32.3 mmoles) of morpholine hydrochloride is heated at 160° C. under a nitrogen atmosphere for 2 and a half hours. The solid mass obtained is dissolved in 200 ml of boiling isopropyl alcohol. The mixture is filtered hot and the filtrate is concentrated until a solid suspension appears. The mixture is then cooled to room temperature and 200 ml of diethyl ether are added. The reaction product crystallizes. It is filtered, washed with diethyl ether and dried. 6.8 g of N-]imino(cyclopropylamino)methyl]-4-morpholinecarboximidamide hydrochloride are obtained. Yield: 85%. M.P.: 195°-196° C.
후처리
- customThe solid mass obtained
- filtrationThe mixture is filtered hot
- concentrationthe filtrate is concentrated until a solid suspension
- temperatureThe mixture is then cooled to room temperature
- addition200 ml of diethyl ether are added
- customThe reaction product crystallizes
- filtrationIt is filtered
- washwashed with diethyl ether
- customdried
출처 및 근거
- ORD 기록
- ord-e9d8d1c4b04e4b0ab4dc23ddc55eab85
- 출처 데이터셋
- uspto-grants-1993_11
- 특허 번호
- US05258513
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