Water → HCID 86665397、化合物

HRID 405675ノート

反応式

HRID 405675 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:5]([NH2:7])=[O:6].C([N:21]=[C:22]=[S:23])(=O)C1C=CC=CC=1.O>CC(C)=O>[CH3:12][O:11][C:10]1[CH:9]=[CH:8][C:4]([C:5]([NH2:7])=[O:6])=[CH:3][C:2]=1[NH:1][C:22]([NH2:21])=[S:23]

参加物

5

反応物 3

HCID 962WaterHCID 68284Benzoyl isothiocyanateHCID 871353-Amino-4-methoxybenzamide

生成物 1

HCID 86665397HCID 86665397、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 3-amino-4-methoxybenzamide (2.49 g, 15.0 mmol, Alfa) in acetone (30 mL) at reflux was added benzoyl isothiocyanate (2.22 mL, 16.5 mmol) and the mixture was stirred at reflux for 30 min, then was poured into water. The precipitate was collected by vacuum filtration and was treated with 10% aq. NaOH (15 mL). The mixture was heated to reflux for 40 min, cooled to room temperature, and poured into a mixture of ice and 6 N aq. HCl. The mixture was basified to pH 10 with conc. aq. NH4OH and the resulting white solid precipitate was collected by vacuum filtration, affording the crude title compound, which was used without further purification.

後処理

  1. temperatureat reflux for 30 min
  2. filtrationThe precipitate was collected by vacuum filtration
  3. additionwas treated with 10% aq. NaOH (15 mL)
  4. temperatureThe mixture was heated
  5. temperatureto reflux for 40 min
  6. additionpoured into a mixture of ice and 6 N aq. HCl
  7. filtrationthe resulting white solid precipitate was collected by vacuum filtration

出典と根拠

ORDレコード
ord-1655a71125cc4700930c4e347551a1b3
出典データセット
uspto-grants-2014_06
特許番号
US08753857B2

反応ノート

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