Thiomorpholine → HCID 5185429, 화합물
반응식
[NH2:1][C:2]1[N:7]([OH:8])[C:6](=[NH:9])[N:5]=[C:4](Cl)[CH:3]=1.[NH:11]1[CH2:16][CH2:15][S:14][CH2:13][CH2:12]1>CN(C)C=O>[NH2:1][C:2]1[N:7]([OH:8])[C:6](=[NH:9])[N:5]=[C:4]([N:11]2[CH2:16][CH2:15][S:14][CH2:13][CH2:12]2)[CH:3]=1참가 물질
4
반응 조건
- 온도
- 110 °C
실험 절차
A mixture of 16.1 g of 6-amino-4-chloro-1,2-dihydro-2-imino-1-pyrimidinol, 32.1 g of thiomorphline, and 75 ml of dimethyl formamide is heated at 110°C in a nitrogen atmosphere for 17 hours. The solvent is removed under high vacuum. The residue is dissolved in 2 normal hydrochloric acid, and the resulting solution made basic with 5% ammonium hydroxide. There is deposited 13.0 g (57%) of a crystalline solid mp 242°(dec). Recrystallization from methanol-ethanol gives an off-white crystalline solid, mp 246°C(dec).
후처리
- customThe solvent is removed under high vacuum
- dissolutionThe residue is dissolved in 2 normal hydrochloric acid
- customRecrystallization from methanol-ethanol
- customgives an off-white crystalline solid, mp 246°C(dec)
출처 및 근거
- ORD 기록
- ord-5971cbac111a4e01b2a733085311e34e
- 출처 데이터셋
- uspto-grants-1976_08
- 특허 번호
- US03973016
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