3-(Trifluoromethyl)phenylcyanamide → HCID 178490592、化合物

HRID 636684

反応式

HRID 636684 の反応式
[NH:1]([C:4]1[CH:5]=[C:6]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:8][CH:9]=1)[C:2]#[N:3].Cl.[CH3:15][O:16][C:17]1[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][C:18]=1[NH2:19]>C(#N)C>[CH3:15][O:16][C:17]1[CH:23]=[CH:22][C:21]([C:24]([F:25])([F:26])[F:27])=[CH:20][C:18]=1[NH:19][C:2]([NH:1][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:11])([F:12])[F:13])[CH:5]=1)=[NH:3]

参加物

4

反応物 2

HCID 110741023-(Trifluoromethyl)phenylcyanamideHCID 700096092-Methoxy-5-(trifluoromethyl)aniline hydrochloride

生成物 1

HCID 178490592HCID 178490592、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 3-cyanamidobenzotrifluoride (0.40 g, 2.15 mmol), 2-methoxy-5-triflouromethylaniline hydrochloric acid salt (0.53 g, 2.33 mmol) and acetonitrile (20 ml) was stirred at reflux for 40 h. The solvent was evaporated. Dichloromethane (50 ml) was added and the mixture was washed with saturated aqueous sodium hydrogen carbonate (50 ml). The organic phase was purified by chromatography using silica gel and a mixture of methanol (10%) and dichloromethane as eluent. The product was isolated as the free base. Yield 0.40 g, 49%. M.p. 45-47° C.

後処理

  1. temperatureat reflux for 40 h
  2. customThe solvent was evaporated
  3. additionDichloromethane (50 ml) was added
  4. washthe mixture was washed with saturated aqueous sodium hydrogen carbonate (50 ml)
  5. customThe organic phase was purified by chromatography
  6. additiona mixture of methanol (10%) and dichloromethane as eluent
  7. customThe product was isolated as the free base

出典と根拠

ORDレコード
ord-8d904f464e7541fe803fbfa70b6cc7c7
出典データセット
uspto-grants-2001_02
特許番号
US06194447B1

関連ノート

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