Acetone → HCID 73186994, 화합물

HRID 986378노트

반응식

HRID 986378 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 73186994HCID 73186994, 화합물수율 52%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
150 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d62eca8db4264c7e88d4b1734a028386
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04713316

반응 노트

불러오는 중…