Trifluoroacetic acid → HCID 18689938、化合物

HRID 1871922ノート

反応式

HRID 1871922 の反応式
C(OC([N:8]1[CH2:13][CH2:12][C:11](=[CH:14][C:15]2[CH:24]=[CH:23][C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[N:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>ClCCl>[N:16]1[C:17]2[C:22](=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:23]=[CH:24][C:15]=1[CH:14]=[C:11]1[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 18689933HCID 18689933、化合物

生成物 1

HCID 18689938HCID 18689938、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-tert-Butoxycarbonyl-4-(2-quinolylmethylene)piperidine (17.6 g) was dissolved in dichloromethane (60 ml), and TFA (60 ml) was added to the solution under cooling on ice. The mixture was stirred for 2.5 hours at room temperature and concentrated under reduced pressure. A saturated solution of sodium hydrogencarbonate was added to the residue to neutralize, and the mixture was then extracted with chloroform. The organic phase was dried over sodium sulfate anhydrate and concentrated under reduced pressure. The title compound was recovered from an etherhexane solvent as white powder. This powder was also used for subsequent reaction without further purification.

後処理

  1. temperatureunder cooling on ice
  2. concentrationconcentrated under reduced pressure
  3. additionA saturated solution of sodium hydrogencarbonate was added to the residue
  4. extractionthe mixture was then extracted with chloroform
  5. dry with materialThe organic phase was dried over sodium sulfate anhydrate
  6. concentrationconcentrated under reduced pressure
  7. customThe title compound was recovered from an etherhexane solvent as white powder
  8. customThis powder was also used for subsequent reaction without further purification

出典と根拠

ORDレコード
ord-608e8741f1bb4b8bb7d3396782077e66
出典データセット
uspto-grants-2000_08
特許番号
US06107308

反応ノート

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