Triethylamine → 1,3-Di(2,2,2-trifluoroethyl)thiourea
反応式
[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]参加物
5
実験手順
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°.
後処理
- 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°)
出典と根拠
- ORDレコード
- ord-291331072b234f3eae842ce3a0c3e233
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04762932
反応ノート
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