Benzyl Isothiocyanate → N-Benzyl-N'-(3-chloro-5-trifluoromethyl-2-pyridyl)methylthiourea

HRID 2416014

반응식

HRID 2416014 반응식
Cl.[Cl:2][C:3]1[C:4]([CH2:13][NH2:14])=[N:5][CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[CH2:15]([N:22]=[C:23]=[S:24])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>O1CCCC1.C(N(CC)CC)C>[CH2:15]([NH:22][C:23]([NH:14][CH2:13][C:4]1[C:3]([Cl:2])=[CH:8][C:7]([C:9]([F:12])([F:10])[F:11])=[CH:6][N:5]=1)=[S:24])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

5

반응물 2

HCID 2346Benzyl IsothiocyanateHCID 114997441-[3-Chloro-5-(trifluoromethyl)pyridin-2-yl]methanamine--hydrogen chloride (1/1)

생성물 1

HCID 22637232N-Benzyl-N'-(3-chloro-5-trifluoromethyl-2-pyridyl)methylthiourea

시약·촉매·용매 2

HCID 8471Triethylamine촉매HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of (3-chloro-5-trifluoromethyl-2-pyridyl)methylamine hydrochloride (0.12 g) and benzylisothiocyanate (0.11 g) in dry tetrahydrofuran (10 ml) was added triethylamine (10 drops) and the mixture stirred at room temperature for 12 hours. The solvent was evaporated and ethyl acetate added. The mixture was washed with 2M hydrochloric acid and then with saturated sodium bicarbonate solution. The organic layer was separated and the solvent removed to give the title product. 1H N.M.R. δ(ppm) 4.7 (2H, broad s), 4.95 (2H, d), 6.9 (1H, broad s), 7.3-7.55 (6H, m), 7.95 (1H, s) and 8.58 (1H, s).

후처리

  1. customThe solvent was evaporated
  2. additionethyl acetate added
  3. washThe mixture was washed with 2M hydrochloric acid
  4. customThe organic layer was separated
  5. customthe solvent removed

출처 및 근거

ORD 기록
ord-28e0e1d6a64047fa93a0ce93b34299c0
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06821992B1

연결된 노트

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