Chlorosulfamic acid → HCID 66747382, 화합물

HRID 711694노트

반응식

HRID 711694 반응식
[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]

참가 물질

5

반응물 2

HCID 24499Chlorosulfamic acidHCID 66745948HCID 66745948, 화합물

생성물 1

HCID 66747382HCID 66747382, 화합물수율 191.1%

시약·촉매·용매 2

HCID 962Water용매HCID 31374Dimethylacetamide용매

실험 절차

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+).

후처리

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

출처 및 근거

ORD 기록
ord-1b2ea7988d8b471f8e30fb2c81afb5e3
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181276B2

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