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

HRID 364303

반응식

HRID 364303 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

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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

  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°)

출처 및 근거

ORD 기록
ord-608fcf617d1f4a088c59ba2a5375b18b
출처 데이터셋
uspto-grants-1986_08
특허 번호
US04604465

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