Triethylamine → 1,3-Di(2,2,2-trifluoroethyl)thiourea
반응식
[F:1][C:2]([F:8])([F:7])[CH2:3][N:4]=[C:5]=[S:6].Cl.[F:10][C:11]([F:15])([F:14])[CH2:12][NH2:13].C(N(CC)CC)C>C(#N)C>[F:1][C:2]([F:8])([F:7])[CH2:3][NH:4][C:5]([NH:13][CH2:12][C:11]([F:15])([F:14])[F:10])=[S:6]참가 물질
5
실험 절차
2,2,2-Trifluoroethylisothiocyanate (2.12 g.) was added to a mixture of 2,2,2-trifluoroethylamine hydrochloride (1.36 g.), triethylamine (1.01 g.) and acetonitrile (10 ml.), and the mixture stirred at room temperature for 4 hours and then evaporated to dryness. The residue was partitioned between water and ethyl acetate, and the ethyl acetate phase was dried and evaporated to dryness. The residue was recrystallised from a mixture of acetone and light petroleum ether (b.p. 60°-80°) to give 1,3-di(2,2,2-trifluoroethyl)thiourea, m.p. 152°-153°.
후처리
- customevaporated to dryness
- customThe residue was partitioned between water and ethyl acetate
- dry with materialthe ethyl acetate phase was dried
- customevaporated to dryness
- customThe residue was recrystallised from a mixture of acetone and light petroleum ether (b.p. 60°-80°)
출처 및 근거
- ORD 기록
- ord-608fcf617d1f4a088c59ba2a5375b18b
- 출처 데이터셋
- uspto-grants-1986_08
- 특허 번호
- US04604465
반응 노트
불러오는 중…