Hydrochloric Acid → 1-(4-Trifluoromethylphenyl)-2-methyl-3-pyrrolidino-1-propanone

HRID 345498

反応式

HRID 345498 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:12])[CH2:10][CH3:11])=[CH:5][CH:4]=1.[CH2:15]=O.Cl.[NH:18]1[CH2:22][CH2:21][CH2:20][CH2:19]1.Cl>>[F:1][C:2]([F:13])([F:14])[C:3]1[CH:4]=[CH:5][C:6]([C:9](=[O:12])[CH:10]([CH3:15])[CH2:11][N:18]2[CH2:22][CH2:21][CH2:20][CH2:19]2)=[CH:7][CH:8]=1

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 136554p-TrifluoromethylpropiophenoneHCID 212848Pyrrolidine, hydrochloride (1:1)

生成物 1

HCID 99477501-(4-Trifluoromethylphenyl)-2-methyl-3-pyrrolidino-1-propanone収率 44.8%

実験手順

A mixture of 1-(4-trifluoromethylphenyl)-1-propanone (2.50g), paraformaldehyde (1.10g), pyrrolidine hydrochloride (1.60g), and hydrochloric acid (0.1 ml) was refluxed for 16 hours. The mixture was evaporated in vacuo to give the residue. The residue was partitioned into water and ethyl acetate. The aqueous layer was neutralized with ammonia water and then extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and then filtered. The filtrate was evaporated in vaccuo to give 1-(4-trifluoromethylphenyl)-2-methyl-3-pyrrolidino-1propanone (1.58g; yield: 44.8%) as an oil.

後処理

  1. temperaturewas refluxed for 16 hours
  2. customThe mixture was evaporated in vacuo
  3. customto give the residue
  4. customThe residue was partitioned into water and ethyl acetate
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customThe filtrate was evaporated in vaccuo

出典と根拠

ORDレコード
ord-6e92e8cdde03423680812f606fb4b53a
出典データセット
uspto-grants-1991_10
特許番号
US05057535

関連ノート

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