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Cyanamide → HCID 178480761、化合物

HRID 1914759
ノート
印刷プレビュー

反応式

HRID 1914759 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:9]=[CH:10][C:11]([O:15][C:16]([F:19])([F:18])[F:17])=[C:12]([NH2:14])[CH:13]=2)[CH2:4][CH2:3]1.[N:20]#[C:21][NH2:22]>Cl.O>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:9]=[CH:10][C:11]([O:15][C:16]([F:19])([F:17])[F:18])=[C:12]([NH:14][C:21]([NH2:22])=[NH:20])[CH:13]=2)[CH2:4][CH2:3]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 9864CyanamideHCID 249941425-(4-Methylpiperazin-1-yl)-2-trifluoromethoxyphenylamine

生成物 1

HCID 178480761HCID 178480761、化合物収率 76%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

To a solution of 5-(4-methyl-piperazin-1-yl)-2-trifluoromethoxy-phenylamine (275 mg, 1 mmol) in HCl 6N (1 mL), cyanamide (336 mg, 8.0 mmol) was added and the reaction was stirred at 60° C. for 1 h. The mixture was cooled down to room temperature, diluted with water (3 mL), extracted with DCM (10 mL). NaOH 2N was added to pH>11. The aqueous phase was extracted with Et2O (3×10 mL), dried over sodium sulfate and concentrated. The residue was crystallized from diethyl ether to give the title compound (240 mg, 76% yield) as a white solid.

後処理

  1. temperatureThe mixture was cooled down to room temperature
  2. extractionextracted with DCM (10 mL)
  3. additionNaOH 2N was added to pH>11
  4. extractionThe aqueous phase was extracted with Et2O (3×10 mL)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue was crystallized from diethyl ether

出典と根拠

ORDレコード
ord-8aca38b3ccb64ca4999b051da1f10def
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08614220B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート