Triethylamine → 1,3-Di(2,2,2-trifluoroethyl)thiourea

HRID 364303

反応式

HRID 364303 の反応式
[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

反応物 3

HCID 8471TriethylamineHCID 97722,2,2-Trifluoroethylamine hydrochlorideHCID 138837771,1,1-Trifluoro-2-isothiocyanatoethane

生成物 1

HCID 117764131,3-Di(2,2,2-trifluoroethyl)thiourea

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

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

  1. customevaporated to dryness
  2. customThe residue was partitioned between water and ethyl acetate
  3. dry with materialthe ethyl acetate phase was dried
  4. customevaporated to dryness
  5. 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-608fcf617d1f4a088c59ba2a5375b18b
出典データセット
uspto-grants-1986_08
特許番号
US04604465

関連ノート

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