Potassium Carbonate → HCID 178484441、化合物

HRID 2172677ノート

反応式

HRID 2172677 の反応式
[C:1]([C:3]1[CH:13]=[CH:12][C:6]([C:7]([N:9]([CH3:11])[CH3:10])=[O:8])=[CH:5][CH:4]=1)#[N:2].C(=O)([O-])[O-].[K+].[K+].Cl.[NH2:21][OH:22]>CCO.CCOC(C)=O>[OH:22][NH:21][C:1]([C:3]1[CH:13]=[CH:12][C:6]([C:7]([N:9]([CH3:11])[CH3:10])=[O:8])=[CH:5][CH:4]=1)=[NH:2]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 162277964-Cyano-N,N-dimethylbenzamide

生成物 1

HCID 178484441HCID 178484441、化合物収率 79%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

4-cyano-N,N-dimethylbenzamide (200 mg, 1.148 mmol), potassium carbonate (952 mg, 6.89 mmol) and hydroxylamine hydrochloride (479 mg, 6.89 mmol) were dissolved in EtOH (11.4 mL). The reaction mixture was stirred at 80° C. for 25 h. The mixture was diluted with EtOAc (50 mL), washed with water (10 mL), water phase extracted with EtOAc (20 mL). Combined organic phases were washed with brine (10 mL) and dried over sodium sulfate. The solvent was removed to give 188 mg of white crystalline needles. The crude material was used without further purification.

後処理

  1. washwashed with water (10 mL), water phase
  2. extractionextracted with EtOAc (20 mL)
  3. washCombined organic phases were washed with brine (10 mL)
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed

出典と根拠

ORDレコード
ord-5d180c150ed044609ff387b770a67238
出典データセット
uspto-grants-2015_06
特許番号
US09056843B2

反応ノート

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