Chlorosulfamic acid → HCID 66747382、化合物

HRID 471557ノート

反応式

HRID 471557 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH:11]([CH3:13])[CH3:12])[C:3]=1[C:4]#[N:5].[S:14](Cl)(=[O:17])(=[O:16])[NH2:15]>CC(N(C)C)=O.O>[S:14]([NH2:1])([NH2:15])(=[O:17])=[O:16].[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH:11]([CH3:13])[CH3:12])[C:3]=1[C:4]#[N:5]

参加物

5

反応物 2

HCID 24499Chlorosulfamic acidHCID 66745948HCID 66745948、化合物

生成物 1

HCID 66747382HCID 66747382、化合物収率 191.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 31374Dimethylacetamide溶媒

実験手順

To a solution of 2-amino-6-(isopropylamino)benzonitrile (Example 90b) (0.09 g, 0.54 mmol) in DMA (3 mL) was added sulfamoyl chloride (0.19 g, 1.62 mmol). The reaction mixture was stirred at room temperature under nitrogen for 2 hours, diluted with H2O (5 mL) and extracted with EtOAc. Solvents of the combined organic phases were evaporated and the residue was purified by preparative thin layer chromatography using a Hexane/EtOAc (3:2) solution as eluant, to give 2-amino-6-(isopropylamino)benzonitrile sulfamide (0.14 g). MS 255 (MH+).

後処理

  1. extractionextracted with EtOAc
  2. customSolvents of the combined organic phases were evaporated
  3. customthe residue was purified by preparative thin layer chromatography

出典と根拠

ORDレコード
ord-18b3d31e373144209e6050baf94784d0
出典データセット
uspto-grants-2014_01
特許番号
US08633186B2

反応ノート

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