2-Bromo-1-indanone → HCID 178419873, 화합물

HRID 865088노트

반응식

HRID 865088 반응식
Br[CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]1=O.Cl.[NH:13]1[CH:17]=[C:16]([CH2:18][C:19]([NH2:21])=[S:20])[N:15]=[CH:14]1>CC(O)C>[NH:13]1[CH:17]=[C:16]([CH2:18][C:19]2[S:20][C:2]3[CH2:10][C:9]4[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=4[C:3]=3[N:21]=2)[N:15]=[CH:14]1

참가 물질

4

반응물 2

HCID 1372032-Bromo-1-indanoneHCID 178479561HCID 178479561, 화합물

생성물 1

HCID 178419873HCID 178419873, 화합물수율 32.4%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

0.34 g of 2-bromo-1-indanone and 0.26 g of 4-imidazolyl thioacetamide hydrochloride were dissolved in 7 ml of 2-propanol with heating, and the solution was heated for 30 minutes under reflux. After cooling the reaction solution, the precipitated crystals were collected by filtration and washed with ethyl acetate. The collected crystals were partitioned between chloroform and a saturated aqueous sodium bicarbonate solution, and the aqueous layer was extracted with chloroform several times. The combined chloroform layers were washed with a saturated aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. By evaporation of the solvent, 0.12 g (32%) of 2-(4-imidazolylmethyl)-8H-indeno[1,2-d]thiazole was obtained. This free base was dissolved in methanol and mixed with 0.055 g of fumaric acid to effect crystallization. The resulting crude crystals were recrystallized from methanol-diethyl ether to obtain 0.10 g of fumarate.

후처리

  1. temperaturewith heating
  2. temperaturethe solution was heated for 30 minutes
  3. temperatureunder reflux
  4. temperatureAfter cooling the reaction solution
  5. filtrationthe precipitated crystals were collected by filtration
  6. washwashed with ethyl acetate
  7. customThe collected crystals were partitioned between chloroform
  8. extractiona saturated aqueous sodium bicarbonate solution, and the aqueous layer was extracted with chloroform several times
  9. washThe combined chloroform layers were washed with a saturated aqueous sodium chloride solution
  10. dry with materialdried over anhydrous magnesium sulfate
  11. customBy evaporation of the solvent

출처 및 근거

ORD 기록
ord-ab4ab6f8264749c59102bfb043a19a79
출처 데이터셋
uspto-grants-1996_10
특허 번호
US05565479

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