Potassium ethylxanthate → HCID 178509644、化合物

HRID 1022769

反応式

HRID 1022769 の反応式
[NH2:1][C:2]1[C:9]([OH:10])=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].C(O[C:14]([S-])=[S:15])C.[K+]>N1C=CC=CC=1>[SH:15][C:14]1[O:10][C:9]2[C:2](=[C:3]([C:4]#[N:5])[CH:6]=[CH:7][CH:8]=2)[N:1]=1

参加物

4

反応物 2

HCID 2735045Potassium ethylxanthateHCID 159063362-Amino-3-hydroxybenzonitrile

生成物 1

HCID 178509644HCID 178509644、化合物収率 45.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 2-amino-3-hydroxybenzonitrile (298 mg) and potassium ethylxanthate (427 mg) in pyridine (7.4 ml) was heated under reflux for 3 hr. To the reaction mixture was added distilled water, the mixture was acidified with 1 M hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with distilled water and brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (178 mg).

後処理

  1. temperatureunder reflux for 3 hr
  2. additionTo the reaction mixture was added
  3. distillationdistilled water
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe extract was washed with distilled water and brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-10ea5d5ffe4d4cfdbb2aa24469c0957c
出典データセット
uspto-grants-2014_05
特許番号
US08722662B2

関連ノート

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