2-Bromo-1-indanone → HCID 178419873、化合物

HRID 865088ノート

反応式

HRID 865088 の反応式
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

参加物

4

反応物 2

HCID 1372032-Bromo-1-indanoneHCID 178479561HCID 178479561、化合物

生成物 1

HCID 178419873HCID 178419873、化合物収率 32.4%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ab4ab6f8264749c59102bfb043a19a79
出典データセット
uspto-grants-1996_10
特許番号
US05565479

反応ノート

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