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Pyrrolidin-1-amine monohydrochloride → 3-(4-Fluorophenyl)-5-isopropyl-2-phenyl-1-(1-pyrrolidinyl)pyrrole

HRID 704744
ノート
印刷プレビュー

反応式

HRID 704744 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH2:17][C:18](=O)[CH:19]([CH3:21])[CH3:20])[C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=O)=[CH:4][CH:3]=1.Cl.[NH2:24][N:25]1[CH2:29][CH2:28][CH2:27][CH2:26]1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:17]=[C:18]([CH:19]([CH3:21])[CH3:20])[N:24]([N:25]3[CH2:29][CH2:28][CH2:27][CH2:26]3)[C:9]=2[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3017392Pyrrolidin-1-amine monohydrochlorideHCID 143002712-(4-Fluorophenyl)-5-methyl-1-phenylhexane-1,4-dione

生成物 1

HCID 145787423-(4-Fluorophenyl)-5-isopropyl-2-phenyl-1-(1-pyrrolidinyl)pyrrole

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

20 g of molecular sieve 3 Å are added to 15 g (50 mmol) of the compound from Example 2 and 20 g (164 mmol) of N-aminopyrrolidine hydrochloride in 150 ml of toluene AR and the mixture is heated to reflux for 48 hours. The mixture is cooled, filtered and washed well with toluene. The toluene solutions are combined and extracted 3×using 1N hydrochloric acid. The organic phase is subsequently washed using saturated sodium hydrogen carbonate solution, dried over magnesium sulphate and concentrated in vacuo. The residue is stirred with a little ethanol, cooled and filtered off with suction. After drying in a desiccator, 2.3 g of substance are obtained.

後処理

  1. temperaturethe mixture is heated
  2. temperatureto reflux for 48 hours
  3. temperatureThe mixture is cooled
  4. filtrationfiltered
  5. washwashed well with toluene
  6. extractionextracted 3×
  7. washThe organic phase is subsequently washed
  8. dry with materialdried over magnesium sulphate
  9. concentrationconcentrated in vacuo
  10. temperaturecooled
  11. filtrationfiltered off with suction
  12. customAfter drying in a desiccator
  13. custom2.3 g of substance are obtained

出典と根拠

ORDレコード
ord-fc405942416745cd910ff6c2d1936186
出典データセット
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04988711

反応ノート

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