Acetone → HCID 73186994、化合物

HRID 986378ノート

反応式

HRID 986378 の反応式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([O-:10])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[Cl:12][C:13]1[CH:14]=[CH:15][C:16]2[S:20][C:19]([CH3:21])=[N+:18]([CH2:22][CH3:23])[C:17]=2[CH:24]=1.[CH3:25]O.[CH3:27][C:28](C)=[O:29]>C(OCC)(=O)C>[C:1]1([CH3:11])[CH:2]=[CH:3][C:4]([S:7]([O-:10])(=[O:8])=[O:9])=[CH:5][CH:6]=1.[Cl:12][C:13]1[CH:14]=[CH:15][C:16]2[S:20][C:19]([CH:21]=[C:28]3[CH:27]=[C:11]([CH3:25])[C:1]4[C:6](=[CH:5][CH:4]=[CH:3][CH:2]=4)[O:29]3)=[N+:18]([CH2:22][CH3:23])[C:17]=2[CH:24]=1

参加物

5

反応物 3

HCID 180AcetoneHCID 887MethanolHCID 1130905-Chloro-3-ethyl-2-methylbenzothiazolium p-toluenesulfonate

生成物 1

HCID 73186994HCID 73186994、化合物収率 52%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
150 °C

実験手順

11.1 g of 5-chloro-3-ethyl-2-methylbenzothiazolium p-toluenesulfonate and 5.5 g of 4-methylcoumarin-2-thione were reacted under heat at 150° C. for 23 hours, and then 25 ml of methanol, 50 ml of acetone and 150 ml of ethyl acetate were added to the reaction mixture in the order listed. After cooling to room temperature, crystals precipitated out from the reaction solution, and the crystals were separated by filtration and washed with a small amount of acetone. Afterwards, the crystals were placed in a mixed solvent comprising 25 ml of methanol, 50 ml of acetone, and 150 ml of ethyl acetate at room temperature, and stirred for 20 minutes, and then the crystals was again separated by filtration and washed with acetone, to finally obtain 7.9 g of the desired p-toluenesulfonate product. Yield: 52%. Appearance: brown crystal. M.p.: 282°-283° C. (decomposition).

後処理

  1. temperatureAfter cooling to room temperature
  2. customcrystals precipitated out from the reaction solution
  3. customthe crystals were separated by filtration
  4. washwashed with a small amount of acetone
  5. customwere placed in a mixed solvent comprising 25 ml of methanol, 50 ml of acetone, and 150 ml of ethyl acetate at room temperature
  6. customthe crystals was again separated by filtration
  7. washwashed with acetone, to finally obtain 7.9 g of the desired p-toluenesulfonate product

出典と根拠

ORDレコード
ord-d62eca8db4264c7e88d4b1734a028386
出典データセット
uspto-grants-1987_12
特許番号
US04713316

反応ノート

読み込み中…