Hydrochloric Acid → HCID 22044636、化合物

HRID 1830486ノート

反応式

HRID 1830486 の反応式
[F:1][C:2]1[C:14]2[CH2:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][C:11]=3[F:15])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].[C:20](Cl)(=[O:23])[CH2:21][CH3:22].Cl>C(=S)=S>[C:20]([C:10]1[CH:9]=[CH:8][C:7]2[C:6]3[C:14](=[C:2]([F:1])[CH:3]=[CH:4][CH:5]=3)[CH2:13][C:12]=2[C:11]=1[F:15])(=[O:23])[CH2:21][CH3:22]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 62324Propionyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 22045596HCID 22045596、化合物

生成物 1

HCID 22044636HCID 22044636、化合物収率 31.8%

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

50.5 g of 1,8-difluorofluorene (K-1) was dissolved in 150 ml of carbon disulfide, and the temperature was lowered to −10° C. With the temperature maintained at this level, 30 g of anhydrous aluminum chloride was added, and with the temperature still held at −10° C., 25.4 g of propionyl chloride was added dropwise over a period of 30 minutes, and the mixture was then stirred at the same temperature for 2 hours. Following completion of the stirring, the reaction mixture was poured into 200 ml of cooled 1N dilute hydrochloric acid, and was then extracted with 250 ml of toluene. The thus obtained organic layer was washed twice with 100 ml portions of water. Following drying, the solvent was removed by evaporation and the product purified by silica gel chromatography (toluene) to yield 20.5 g of 2-propionyl-1,8-difluorofluorene (K-2).

後処理

  1. customwas lowered to −10° C
  2. additionwas added
  3. customstill held at −10° C.
  4. extractionwas then extracted with 250 ml of toluene
  5. washThe thus obtained organic layer was washed twice with 100 ml portions of water
  6. customFollowing drying
  7. customthe solvent was removed by evaporation
  8. customthe product purified by silica gel chromatography (toluene)

出典と根拠

ORDレコード
ord-396f4ac0ba8b4fdcaedb3b5a088b3bb0
出典データセット
uspto-grants-2006_06
特許番号
US07067179B1

反応ノート

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