Water → HCID 178456349、化合物

HRID 1619236ノート

反応式

HRID 1619236 の反応式
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[S:11][C:12]3[CH:18]=[C:17]([C:19]#[N:20])[CH:16]=[CH:15][C:13]=3[N:14]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].Cl.[NH2:22][OH:23].O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[OH:23][NH:22][C:19]([C:17]1[CH:16]=[CH:15][C:13]2[N:14]=[C:10]([N:7]3[CH2:6][CH2:5][N:4]([CH:1]([CH3:2])[CH3:3])[CH2:9][CH2:8]3)[S:11][C:12]=2[CH:18]=1)=[NH:20]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 237287892-(4-Isopropylpiperazin-1-yl)benzothiazole-6-carbonitrile

生成物 1

HCID 178456349HCID 178456349、化合物収率 71.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2-(4-isopropylpiperazin-1-yl)benzothiazole-6-carbonitrile (5.0 g, 17.5 mmol) in ethanol (50 mL) was added hydroxylamine hydrochloride (3.6 g, 52.4 mmol), water (8 mL) and potassium carbonate (7.2 g, 52.4 mmol). The reaction mixture was heated overnight at reflux. The mixture was allowed to cool and then concentrated in vacuo. The residue was dissolved into THF (30 mL) and then filtered. The filtrate was concentrated in vacuo to give 4 g of crude N-hydroxy-2-(4-isopropylpiperazin-1-yl)benzothiazole-6-carboxamidine.

後処理

  1. temperatureThe reaction mixture was heated overnight
  2. temperatureat reflux
  3. temperatureto cool
  4. concentrationconcentrated in vacuo
  5. dissolutionThe residue was dissolved into THF (30 mL)
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-9c677b7b54c44bd2970b6a1a09cb9736
出典データセット
uspto-grants-2014_07
特許番号
US08772285B2

反応ノート

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